CN115846624B - Preparation method of ceramic/iron-based honeycomb structural composite material - Google Patents
Preparation method of ceramic/iron-based honeycomb structural composite material Download PDFInfo
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Abstract
The invention discloses a preparation method of a ceramic/iron-based honeycomb structural composite material, and belongs to the technical field of metal matrix composite materials. The method comprises the steps of uniformly mixing sol prepared from ferric nitrate nonahydrate, citric acid and the like with sol prepared from hydrated titanium dioxide, active 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, curing to form a preform, and casting a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb structure composite material. The titanium carbonitride ceramic is uniformly dispersed in the iron matrix of the composite region, the honeycomb wall of the configuration composite material is composed of the composite region with higher hardness, the abrasion action of the honeycomb holes with softer hardness can be obviously reduced, the abrasion resistance is improved by more than 4 times compared with that of the traditional iron and steel materials, 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 structural composite material, and belongs to the technical field of metal matrix composite materials.
Background
In the fields of mines, metallurgy, building materials and the like, wear-resistant parts such as plate hammers, hammer heads, grinding rolls and the like are required to be made of materials with high mechanical and wear-resistant properties. The ceramic/steel-based honeycomb composite material has the advantages of high designability, good wear resistance, low cost and the like, and has become an important development direction of wear-resistant materials for equipment manufacturing.
In a ceramic phase commonly used for ceramic/iron-based composite materials, titanium carbonitride (Ti (C, N)), titanium carbide (TiC), tungsten carbide (WC) and the like are carbonizedAlumina (Al) 2 O 3 ) The oxides such as Zirconia Toughened Alumina (ZTA) and the like have good mechanical and abrasion resistance, and a great deal of research and application work is carried out on the composite materials by students at home and abroad, wherein titanium carbonitride (Ti (C, N)) ceramics have good toughness and low cost, and the composite materials are widely applied to abrasion-resistant parts. However, the wear-resistant part is used for crushing and grinding materials by utilizing extrusion action in service, and the reinforcing 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 self-generated ceramic particles and the iron matrix is also higher, so that the research and development of the in-situ self-generated titanium carbonitride/iron-based composite material are paid attention to by scientific researchers at home and abroad, but no breakthrough progress is made. In addition, the impregnation depth of the iron matrix to the ceramic is insufficient in the preparation process of the traditional ceramic reinforced iron-based surface composite material, the thickness of the composite layer is thin, and the composite layer is easy to peel off in a whole layer when in use due to the large difference of thermophysical parameters of the composite region and the matrix region.
Only chinese patent No. CN202210462248.4 discloses a method for preparing an impeller made of iron-based composite material and synergistically reinforced by titanium carbonitride and chromium carbide, namely, weighing reinforcing body particles and EPS beads according to volume fraction, firstly mixing organic binder with EPS beads, then adding the mixed reinforcing body after mixing, obtaining loose materials with the mixed reinforcing body adhered on the surface of EPS beads, adding the loose materials into a conveying pipe, and preparing the impeller by adopting V-EPC lost foam casting technology. The iron-based composite material prepared by the method has the advantages that the ceramic phase is compounded in an externally added mode, the problem of intrinsic brittleness of the ceramic is not solved, and the ceramic reinforcement and the EPS beads of the polymer are difficult to uniformly disperse due to overlarge density phase difference, so that aggregation segregation and the like are easy to occur.
Disclosure of Invention
In order to solve the problems that the ceramic reinforced iron-based composite material is externally added with large-size ceramic phase intrinsic brittleness, ceramic reinforcement aggregation segregation, easy whole layer peeling of a surface composite material composite region in the service process and insufficient wear resistance, the invention uniformly mixes an iron precursor and a titanium carbonitride precursor to obtain a novel preparation method of a honeycomb composite material with uniformly dispersed ceramic reinforcement in the composite region, and specifically comprises the following steps:
(1) And (3) dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the proportion of the ferric nitrate nonahydrate to the citric acid in the solution, and then placing the mixed solution into a water bath kettle for constant-temperature heating to obtain sol (1).
(2) Adding nano active 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 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, roasting to obtain mixed powder of titanium carbonitride and ferric oxide, and then placing the mixed powder into a reduction furnace for reduction by reducing gas to obtain mixed powder of titanium carbonitride and ferric oxide;
(5) And (3) uniformly stirring the mixed powder obtained in the step (4) and a binder, filling the mixed powder into the honeycomb wall of a honeycomb structure die, solidifying to form a preform, and pouring a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb structure composite material.
Preferably, in the step (1), the molar ratio of the ferric nitrate to the citric acid is 1 (0.6-1.2).
Preferably, the heating conditions of the water bath kettle in the step (1) are as follows: heating at 60-90deg.C for 8-12 hr.
Preferably, the molar ratio of the hydrated titanium dioxide to the nano activated carbon in the step (2) is 1 (0.8-1.2), and the granularity of the nano activated carbon is 10-30nm.
Preferably, the heating conditions of the water bath kettle in the step (2) are as follows: heating at 40-70deg.C for 4-8 hr.
Preferably, in the step (3), the molar ratio of Fe ions in the sol (1) to Ti ions in the sol (2) is 1 (0.02-0.4).
Preferably, the drying conditions in step (3) of the present invention are: drying in vacuum drying oven at 100-150deg.C for 14-20 hr.
Preferably, the calcination and calcination 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 flow rate of the hydrogen is 1.0-2.0m 3 And/h, wherein the time is 4-6h.
Preferably, the binder in the step (5) is any one of polyvinyl alcohol, ethylene-vinyl acetate copolymer and starch paste.
Preferably, in the step (5), the molar ratio of the binder to the mixed powder of titanium carbonitride and iron is (0.02-0.04): 1.
Preferably, the curing conditions in step (5) of the present invention are: curing for 6-10h at 90-130 ℃ in an incubator.
The steel melt is conventional steel, 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 preparing the composite material, so that the problem of reinforcement agglomeration or segregation caused by overlarge density difference when an externally added ceramic reinforcement is mixed with iron or EPS is avoided; 2) In the method, the titanium carbonitride ceramic is in-situ autogenous, the size of the ceramic reinforcement is nano-scale, the intrinsic brittleness of the ceramic is obviously reduced, and the ceramic reinforcement is nucleated and grown in the iron matrix, so that the surface of the reinforcement is pollution-free, and the compatibility between the matrix and the reinforcement is good; 3) The honeycomb wall of the honeycomb composite material is composed of a composite region composed of ceramic and iron with higher hardness, the honeycomb holes are composed of a steel metal region with lower hardness, the composite region with higher hardness can prevent the abrasion of the metal region with lower hardness in the abrasion process, the composite layer is not easy to peel off, and the abrasion resistance is improved by more than 2 times compared with that of the traditional surface composite material and more than 4 times compared with that of the traditional steel material.
Drawings
FIG. 1 is a photograph of a cured honeycomb preform made in accordance with the present invention;
FIG. 2 is a surface morphology of a titanium carbonitride/iron-based honeycomb structured composite material prepared in accordance with the present invention.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by persons skilled in the art without making creative efforts based on the embodiments of the present invention are within 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 structural composite material, which comprises the following specific steps:
(1) And (3) 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 1:1, and then placing the mixed solution into a water bath kettle, and heating at the constant temperature of 80 ℃ for 10 hours to obtain sol (1).
(2) Adding active carbon with 20nm granularity into the hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nanometer active carbon is 1:1, stirring at a high speed, and then placing the mixed solution into a water bath kettle, and heating at a constant temperature of 60 ℃ for 5 hours 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 of 1:0.2, and then placing the mixture into a vacuum drying oven and drying at 105 ℃ for 16 hours to obtain mixed gel.
(4) Calcining the mixed gel obtained in the step (3) for 2.5 hours at 1500 ℃ in nitrogen atmosphere, and then calcining for 4.5 hours at 900 ℃ in air atmosphere to obtain 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 hydrogen is used as a raw materialThe air flow rate was 1.2m 3 And (3) h, wherein the time is 5h, and the mixed powder of titanium carbonitride and iron is obtained.
(6) Uniformly mixing the mixed powder with a polyvinyl alcohol binder, wherein the molar ratio of the polyvinyl alcohol to the mixed powder is 0.02:1, curing for 8 hours at 120 ℃ to form a honeycomb-shaped preform, and a macroscopic photograph of the preform is shown in fig. 1, and as can be seen from fig. 1, titanium carbonitride and iron in the preform are uniformly mixed.
(7) The prefabricated body is placed in a casting cavity, then a smelted high-chromium cast iron melt is poured, after cooling, the titanium carbonitride ceramic/high-chromium cast iron-based honeycomb structural composite material can be obtained, a macroscopic photograph of the structural composite material is shown in fig. 2, the structural composite material is composed of a composite region and a metal region, the honeycomb structure is not dispersed, wherein titanium carbonitride reinforcement bodies in the composite region are uniformly dispersed and distributed in a matrix, no agglomeration phenomenon exists, and no obvious defect exists in the composite region.
The titanium carbonitride reinforced high-chromium cast iron-based honeycomb structural composite material (volume abrasion rate 70.7 mm) 3 And/h), the wear resistance is higher than that of the traditional high-chromium cast iron (the volume wear rate is 290mm 3 And/h) is improved by 4.1 times, compared with the whole layer of composite titanium carbonitride reinforced high-chromium cast iron-based composite material (the volume abrasion rate is 155.5 mm) 3 And/h) is increased by a factor of 2.2.
Example 2
The embodiment relates to a preparation method of a ceramic/high manganese steel-based honeycomb structural composite material, which comprises the following specific steps:
(1) And (3) 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 1:0.6, and then placing the mixed solution into a water bath kettle, and heating at the constant temperature of 60 ℃ for 12 hours to obtain sol (1).
(2) Adding active carbon with the granularity of 10nm into a hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nanometer active carbon is 1:1.2, stirring at a high speed, then placing the mixed solution into a water bath kettle, and heating at the constant temperature of 70 ℃ for 4 hours 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 of 1:0.4, and then placing the mixture into a vacuum drying oven and drying the mixture at 150 ℃ for 14h to obtain mixed gel.
(4) Calcining the mixed gel obtained in the step (3) for 4 hours at 1400 ℃ in nitrogen atmosphere, and then calcining for 3 hours at 1000 ℃ in air atmosphere to obtain mixed powder of titanium carbonitride and ferric oxide.
(5) Placing 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 (3) h, wherein the time is 4h, and the mixed powder of titanium carbonitride and iron is obtained.
(6) And uniformly mixing the mixed powder with an ethylene-vinyl acetate copolymer binder, wherein the mol ratio of the ethylene-vinyl acetate copolymer to the mixed powder is 0.04:1, and curing for 6 hours at 130 ℃ to form the honeycomb-shaped preform.
(7) And (3) placing the preform into a casting cavity, then casting a smelted high manganese steel melt, and cooling to obtain the titanium carbonitride ceramic/high manganese steel-based honeycomb structural composite material.
The titanium carbonitride reinforced high manganese steel based honeycomb structural composite material (volume abrasion rate 60.2 mm) 3 The wear resistance is higher than that of the traditional high manganese steel (the volume wear rate is 240.6 mm) 3 The ratio of the titanium carbonitride to the manganese steel is increased by 4 times, compared with the whole layer of the composite titanium carbonitride reinforced high manganese steel-based composite material (the volume abrasion rate is 126.4 mm) 3 And/h) is increased by a factor of 2.1.
Example 3
The embodiment relates to a preparation method of a ceramic/alloy steel-based honeycomb structural composite material, which comprises the following specific steps:
(1) And (3) 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 1:1.2, and then placing the mixed solution into a water bath kettle, and heating at the constant temperature of 90 ℃ for 8 hours to obtain sol (1).
(2) Adding active carbon with the granularity of 30nm into a hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nanometer active carbon is 1:0.8, stirring at a high speed, and then placing the mixed solution into a water bath kettle, and heating at the constant temperature of 40 ℃ for 8 hours 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 of 1:0.02, and then placing the mixture into a vacuum drying oven and drying at 100 ℃ for 20 hours to obtain mixed gel.
(4) Calcining the mixed gel obtained in the step (3) for 2 hours at 1600 ℃ in nitrogen atmosphere, and then calcining for 5 hours at 800 ℃ in air atmosphere to obtain 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 (3) h, wherein the time is 6h, and the mixed powder of titanium carbonitride and iron is obtained.
(6) And uniformly mixing the mixed powder with an ethylene-vinyl acetate copolymer binder, wherein the mol ratio of the ethylene-vinyl acetate copolymer to the mixed powder is 0.03:1, and curing the mixture at 90 ℃ for 10 hours to form the honeycomb-shaped preform.
(7) And (3) placing the preform into a casting cavity, then casting a smelted alloy steel melt, and cooling to obtain the titanium carbonitride ceramic/alloy steel based honeycomb composite material.
The titanium carbonitride reinforced alloy steel-based honeycomb structural composite material (volume abrasion rate 86.4 mm) 3 And/h), the wear resistance is higher than that of the traditional alloy steel (volume wear rate 362.7 mm) 3 And/h) is improved by 4.2 times, compared with the whole layer of composite titanium carbonitride reinforced alloy steel matrix composite material (the volume abrasion rate is 172.8 mm) 3 And/h) is improved by 2 times.
Example 4
The embodiment relates to a preparation method of a ceramic reinforced high-chromium cast iron-based honeycomb structural composite material, which comprises the following specific steps:
(1) And (3) 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 1:0.8, and then placing the mixed solution into a water bath kettle, and heating at a constant temperature of 75 ℃ for 9.5 hours to obtain sol (1).
(2) Adding active carbon with the granularity of 25nm into a hydrated titanium dioxide solution, wherein the molar ratio of the hydrated titanium dioxide to the nanometer active carbon is 1:1.1, stirring at a high speed, and then placing the mixed solution into a water bath kettle, and heating at a constant temperature of 55 ℃ for 6.5 hours 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 of 1:0.13, and then placing the mixture into a vacuum drying oven and drying at 125 ℃ for 13h to obtain mixed gel.
(4) Calcining the mixed gel obtained in the step (3) for 3.5 hours at 1450 ℃ in nitrogen atmosphere, and then calcining for 2.5 hours at 950 ℃ in air atmosphere to obtain mixed powder of titanium carbonitride and ferric oxide.
(5) The mixed powder is put into a hydrogen reduction furnace, the temperature of the hydrogen reduction furnace is 650 ℃, and the hydrogen flow is 1.4m 3 And (3) h, wherein the time is 5.5h, and the mixed powder of titanium carbonitride and iron is obtained.
(6) And uniformly mixing the mixed powder with a starch paste binder, wherein the molar ratio of the starch paste to the mixed powder is 0.025:1, and curing at 1150 ℃ for 7.5 hours to form the honeycomb-shaped preform.
(7) And (3) placing the preform into a casting cavity, then casting a smelted high-chromium cast iron melt, and cooling to obtain the titanium carbonitride ceramic/high-chromium cast iron-based honeycomb structural composite material.
The titanium carbonitride reinforced high-chromium cast iron-based honeycomb structural composite material (volume abrasion rate 72.5 mm) 3 And/h), the wear resistance is higher than that of the traditional high-chromium cast iron (the volume wear rate is 290mm 3 And/h) is improved by 4 times, compared with the whole layer of composite titanium carbonitride reinforced high-chromium cast iron-based composite material (the volume abrasion rate is 155.5 mm) 3 And/h) is increased by a factor of 2.1.
Claims (8)
1. The preparation method of the ceramic/iron-based honeycomb structural composite material is characterized by comprising the following steps of:
(1) Dissolving ferric nitrate nonahydrate in a citric acid solution, controlling the proportion of the ferric nitrate nonahydrate to the citric acid in the solution, and then placing the mixed solution into a water bath kettle for constant-temperature heating to obtain sol (1);
(2) Adding nano active 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 sol (2);
(3) Uniformly mixing the sol (1) obtained in the step (1) and the sol (2) obtained in the step (2) according to a 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, roasting to obtain mixed powder of titanium carbonitride and ferric oxide, and then placing the mixed powder into a reduction furnace for reduction by reducing gas to obtain mixed powder of titanium carbonitride and ferric oxide;
(5) Uniformly stirring the mixed powder obtained in the step (4) and a binder, filling the mixed powder into the honeycomb wall of a honeycomb structure die, solidifying the mixed powder to form a preform, and pouring a steel melt to obtain the titanium carbonitride ceramic reinforced iron-based honeycomb structure composite material;
the molar ratio of the ferric nitrate to the citric acid in the step (1) is 1 (0.6-1.2);
the molar ratio of the hydrated titanium dioxide to the nanometer activated carbon in the step (2) is 1 (0.8-1.2);
the molar ratio of Fe ions in the sol (1) to Ti ions in the sol (2) is 1 (0.02-0.4);
and (5) the mol ratio of the binder to the mixed powder of titanium carbonitride and iron is (0.02-0.04) 1.
2. The method for preparing the ceramic/iron-based honeycomb structural composite material according to claim 1, wherein the method comprises the following steps: the heating conditions of the water bath kettle in the step (1) are as follows: heating at 60-90deg.C for 8-12 hr.
3. The method for preparing the ceramic/iron-based honeycomb structural composite material according to claim 1, wherein the method comprises the following steps: the granularity of the nano activated carbon in the step (2) is 10-30nm.
4. A method of preparing a ceramic/iron-based honeycomb structured composite according to claim 1 or 3, characterized by: the heating conditions of the water bath kettle in the step (2) are as follows: heating at 40-70deg.C for 4-8 hr.
5. The method for preparing the ceramic/iron-based honeycomb structural 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 vacuum drying oven at 100-150deg.C for 14-20 hr.
6. The method for preparing the ceramic/iron-based honeycomb structural 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 2-4 hr in nitrogen atmosphere and calcining at 800-1000 deg.C for 3-5 hr in air atmosphere.
7. The method for preparing the ceramic/iron-based honeycomb structural composite material according to claim 1, wherein the method comprises the following steps: the reducing gas used in the reducing process in the step (4) is hydrogen, the temperature of the reducing furnace is 600-800 ℃, and the flow of the hydrogen is 1.0-2.0m 3 And/h, wherein the time is 4-6h.
8. The method for preparing the ceramic/iron-based honeycomb structural 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 curing conditions are as follows: curing for 6-10h at 90-130 ℃ in an incubator.
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