CN113862548B - Preparation method of in-situ synthesized ZTA particle reinforced steel-based configuration composite material - Google Patents
Preparation method of in-situ synthesized ZTA particle reinforced steel-based configuration composite material Download PDFInfo
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- B22F3/11—Making porous workpieces or articles
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Abstract
The invention discloses a preparation method of an in-situ synthesized ZTA particle reinforced steel-based configuration composite material, and belongs to the technical field of metal-based composite materials. Preparing transparent sol by using aluminum nitrate nonahydrate, zirconyl nitrate hydrate and the like as raw materials; adding steel-based powder into the sol for liquid-solid doping, stirring until the mixture is solidified, and then sequentially carrying out vacuum drying and reduction on ZTA/steel mixed powder; the ZTA/steel mixed powder is filled into the honeycomb wall of a honeycomb mould, the steel-based powder is filled into the honeycomb hole of the honeycomb mould, and the in-situ authigenic ZTA ceramic particle reinforced steel-based honeycomb-structure composite material can be obtained after pressing and sintering. The ZTA ceramic is generated in situ, the surface of the ceramic particle is pollution-free, the compatibility with a steel matrix is good, and the interface bonding strength is high; the honeycomb wall is composed of a composite area with higher hardness, the abrasion effect on the honeycomb holes with softer hardness can be obviously reduced, the abrasion resistance is improved by more than 3 times compared with the traditional steel material, and the honeycomb wall has wide application prospect.
Description
Technical Field
The invention relates to a preparation method of an in-situ synthesized ZTA particle reinforced steel-based configuration composite material, belonging to the technical field of metal-based composite materials.
Background
The ceramic particle reinforced steel-iron based composite material has become a focus of attention in the scientific research and industrialization fields at home and abroad at present due to the fact that the ceramic particle reinforced steel-iron based composite material has high hardness and high wear resistance of a ceramic material and high strength, good plasticity and toughness of metal. The Zirconia Toughened Alumina (ZTA) ceramic particles have the advantages of good obdurability, high wear resistance, low component content and the like, and the steel-based composite material prepared by the Zirconia Toughened Alumina (ZTA) ceramic particles has excellent wear resistance, and is a research hotspot in the field of the current wear-resistant materials.
But the wetting angle between the ZTA ceramic particles and iron is 130-140 degrees, and the particles are basically not wetted. At home and abroad, relevant researches on non-infiltration type ceramic particle reinforced steel-based composite materials, such as adding an activating element into a steel matrix, plating metal on the surface of particles to improve wettability and the like, interface bonding modes between ceramic particles and the steel matrix in the composite materials prepared by the methods are still mechanical bonding, the bonding strength is low, and the mechanical properties of the composite materials are poor. In addition, the traditional ZTA particle reinforced iron-based surface layer composite material has insufficient impregnation depth of an iron matrix to ZTA ceramic 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 two factors lead to the rapid reduction of the reliability and the wear resistance of the composite material in the wear-resistant service process; if the technical bottleneck is broken through and the wear resistance of the material is improved, the service life of the equipment can be obviously prolonged.
Disclosure of Invention
In order to solve the problems of poor wettability of ZTA ceramic particles and a steel melt, low interface bonding strength, easy whole layer peeling of a surface composite material composite area in the using process and insufficient wear resistance, the invention aims to provide a preparation method of an in-situ synthesized ZTA particle reinforced steel-based configuration composite material, the composite material is a honeycomb-shaped macro-isomerism composite material, and the preparation method specifically comprises the following steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate in deionized water, dripping citric acid to obtain a mixed solution, adjusting the pH value of the mixed solution to be 1-3, adding ethylene glycol, fully stirring, and heating in a constant-temperature water bath kettle to obtain the transparent sol.
(2) Adding iron and steel-based powder into the transparent sol, quickly stirring until the solution is completely solidified (generally 0.1-0.4 h), and then drying under a vacuum condition to obtain ZTA/Fe2O3And (3) mixing the powder, and putting the mixed powder into a reducing furnace to be reduced by reducing gas to obtain ZTA/steel mixed powder.
(3) And filling the ZTA/steel mixed powder into the honeycomb wall of a honeycomb mould, filling the steel-based powder into the honeycomb hole of the honeycomb mould, and pressing and sintering to obtain the in-situ authigenic ZTA ceramic particle reinforced steel-based composite material.
Preferably, the molar ratio of the aluminum nitrate nonahydrate, the zirconyl nitrate hydrate and the citric acid in the mixed solution in the step (1) of the present invention is 1 (0.1 to 0.3) to (0.1 to 0.26), and the molar percentage of the ethylene glycol added to the mixed solution after the pH adjustment is 0.5 to 2.0% (the molar percentage is the ratio of the molar amount of the ethylene glycol to the sum of the molar amounts of the aluminum nitrate nonahydrate, the zirconyl nitrate hydrate and the citric acid).
Preferably, in step (1) of the present invention, the pH of the mixed solution is adjusted by using nitric acid and aqueous ammonia together.
Preferably, the heating conditions in the constant-temperature water bath kettle in the step (1) of the invention are as follows: heating for 6-10 h at 60-90 ℃.
Preferably, the steel-based powder in the step (2) is high-chromium cast iron, high-manganese steel or alloy steel powder, the particle size of the powder is 20-100 microns, and the molar ratio of the steel-based powder to the transparent sol in the step (2) is (0.3-0.7): 1 (the molar ratio is the ratio of the molar weight of the steel-based powder to the sum of the molar weights of all substances forming the sol).
Preferably, the drying conditions under vacuum in step (2) of the present invention are: drying the mixture for 10 to 16 hours in a vacuum drying oven at the temperature of between 100 and 140 ℃.
Preferably, the reducing gas used in the reducing process in the step (2) is hydrogen, the temperature of the reducing furnace is 600-800 ℃, and the flow rate of the hydrogen is 1.0-2.0 m3The time is 5-8 h.
Preferably, the sintering temperature in the step (3) is 900-1400 ℃, and the time is 2-8 h.
The pressing and sintering mode of the invention can be any one of cold isostatic pressing and air furnace sintering, hot isostatic pressing sintering, rapid sintering or spark plasma sintering.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the method, ZTA (zirconia toughened alumina) ceramic particles are in-situ self-generated, the complicated particle surface pretreatment procedure of the traditional externally added ceramic particle reinforcement is avoided, the production efficiency is greatly improved, and the ZTA reinforcement is nucleated and grown in a steel matrix, so that the surfaces of the ceramic particles are free from pollution, the compatibility between the matrix and the particles is good, and the interface bonding strength is higher.
(2) The honeycomb wall of the honeycomb-shaped macro-heterogeneous composite material is composed of the composite zone with higher hardness, the honeycomb holes are composed of the metal zone with lower hardness, in the abrasion process, the composite zone with higher hardness can prevent the abrasion of the metal matrix with lower hardness, the toughness of the metal material and the abrasion resistance of ceramic particles are integrated, the composite layer is not easy to peel off, and the abrasion resistance is improved by more than 3 times compared with the traditional steel material.
Drawings
FIG. 1 is an in-situ autogenous ZTA/high chromium cast iron mixed powder prepared by the present invention;
FIG. 2 is a schematic view of a honeycomb-shaped macro-heterogeneous composite mold according to the present invention;
FIG. 3 is a microstructure diagram of a composite zone of a cellular macro-heterogeneous composite material prepared by the present invention;
fig. 4 is a schematic view of the wear of each area during the wear of the honeycomb-shaped macro-heterogeneous composite material prepared by 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 an in-situ synthesized ZTA ceramic particle reinforced high-chromium cast iron based honeycomb-shaped macro-isomerism composite material, which comprises the following specific steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate in deionized water, and then dripping citric acid to obtain a mixed solution, wherein the molar ratio of the aluminum nitrate nonahydrate to the zirconyl nitrate hydrate to the citric acid is 1:0.1: 0.1.
(2) Adjusting the pH value of the mixed solution to 2 by using nitric acid and ammonia water, adding 1.0 percent (mole fraction) of glycol serving as a dispersing agent into the mixed solution, fully stirring, and then putting into a constant-temperature water bath kettle to heat for 8 hours to obtain transparent sol with certain viscosity.
(3) Adding high-chromium cast iron powder with the particle size of 50 mu m into the sol, wherein the molar ratio of the high-chromium cast iron powder to the transparent sol is 0.5:1, quickly stirring for 0.2h until the high-chromium cast iron powder is completely solidified, then putting the high-chromium cast iron powder into a vacuum drying oven, wherein the temperature of the vacuum drying oven is 120 ℃, and the drying time is 12h to obtain ZTA/Fe2O3Mixing the powder, and putting the mixed powder into a hydrogen reduction furnace with the temperature of 700 ℃ and the hydrogen flow of 1.5m3And h, the time is 6h, and the mixed powder of the ZTA/high-chromium cast iron is obtained, as shown in figure 1, as can be seen from figure 1, the mixed powder of the in-situ synthesized ZTA and the high-chromium cast iron can be obtained by adopting the method, the uniformity of the particle size of the powder is better, the surface of the ceramic particle is free from pollution, and the compatibility between the matrix and the particle is good.
(4) The ZTA/high-chromium cast iron mixed powder is filled into a honeycomb wall of a honeycomb mould, high-chromium cast iron powder is filled into a honeycomb hole of the honeycomb mould, a schematic diagram of the honeycomb macro-isomeric composite material mould is shown in figure 2, the in-situ self-generated ZTA ceramic particles reinforced high-chromium cast iron base honeycomb macro-isomeric composite material can be obtained after cold isostatic pressing and air furnace sintering (sintering temperature is 1400 ℃ and time is 4 hours), a microstructure diagram of a composite area is shown in figure 3, as can be seen from figure 3, in-situ self-generated ZTA ceramic particles in the composite area of the composite material are uniformly dispersed and distributed, no obvious defect exists in the composite area, and impurities exist between the ceramic particles and a micro interface between an iron base body and the interface is well combined.
The wear resistance of the in-situ synthesized ZTA ceramic particle reinforced high-chromium cast iron based honeycomb-shaped macro-isomerism composite material prepared by the invention is improved by 5 times compared with the traditional high-chromium cast iron, the wear schematic diagram is shown in figure 4, and as can be seen from figure 4, because the honeycomb wall composite zone is composed of a high-chromium cast iron matrix and high-hardness ZTA ceramic particles which are dispersedly distributed in the high-chromium cast iron matrix (shown as the position of the part I in the figure), the macro hardness of the honeycomb wall composite zone is obviously higher than that of a honeycomb hole matrix (shown as the position of the part II in the figure), in the wear process, the honeycomb hole with lower hardness is worn firstly, the honeycomb wall with high hardness is worn less, and in the wear direction, the composite zone with higher hardness can protect the wear of the matrix with lower hardness, thereby improving the wear resistance of the material and prolonging the service life.
Example 2
The embodiment relates to a preparation method of an in-situ synthesized ZTA ceramic particle reinforced high manganese steel-based honeycomb-shaped macro-isomerism composite material, which comprises the following specific steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate in deionized water, and then dripping citric acid to obtain a mixed solution, wherein the molar ratio of the aluminum nitrate nonahydrate to the zirconyl nitrate hydrate to the citric acid is 1:0.2: 0.15.
(2) Adjusting the pH value of the mixed solution to 1 by using nitric acid and ammonia water, adding 0.5 percent (mole fraction) of glycol serving as a dispersing agent into the mixed solution, fully stirring, and then putting the mixed solution into a constant-temperature water bath kettle to heat for 6 hours to obtain transparent sol with certain viscosity.
(3) Adding high manganese steel powder with the particle size of 20 mu m into the sol, wherein the molar ratio of the high manganese steel powder to the transparent sol is 0.3:1, quickly stirring for 0.1h until the high manganese steel powder is completely solidified, then putting the high manganese steel powder into a vacuum drying oven, wherein the temperature of the vacuum drying oven is 100 ℃, and the drying time is 16h to obtain ZTA/Fe2O3Mixing the powder, and putting the mixed powder into a hydrogen reduction furnace with the temperature of 600 ℃ and the hydrogen flow of 1.0m3And/h, the time is 5h, and the ZTA/high manganese steel mixed powder is obtained.
(4) Filling the ZTA/high manganese steel mixed powder into the honeycomb wall of a honeycomb-shaped die, filling high manganese steel powder into the honeycomb holes of the honeycomb-shaped die, and performing hot isostatic pressing and sintering (the sintering temperature is 900 ℃ and the time is 8 hours) to obtain the in-situ self-generated ZTA ceramic particle reinforced high manganese steel-based honeycomb-shaped macro-heterogeneous composite material.
The wear resistance of the in-situ synthesized ZTA ceramic particle reinforced high manganese steel-based honeycomb-shaped macro-isomerism composite material prepared by the method is improved by 3 times compared with that of the traditional high manganese steel.
Example 3
The embodiment relates to a preparation method of an in-situ synthesized ZTA ceramic particle reinforced alloy steel base honeycomb-shaped macro-isomerism composite material, which comprises the following specific steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate in deionized water, and then dripping citric acid to obtain a mixed solution, wherein the molar ratio of the aluminum nitrate nonahydrate to the zirconyl nitrate hydrate to the citric acid is 1:0.3: 0.2.
(2) Adjusting the pH value of the mixed solution to 3 by using nitric acid and ammonia water, adding 2.0 percent (mole fraction) of glycol serving as a dispersing agent into the mixed solution, fully stirring, and then putting into a constant-temperature water bath kettle to heat for 10 hours to obtain transparent sol with certain viscosity.
(3) Adding alloy steel powder with the particle size of 100 mu m into the sol, wherein the molar ratio of the alloy steel powder to the transparent sol is 0.6:1, quickly stirring for 0.4h until the mixture is completely solidified, then putting the mixture into a vacuum drying oven, wherein the temperature of the vacuum drying oven is 140 ℃, and the drying time is 10h to obtain ZTA/Fe2O3Mixing the powder, and putting the mixed powder into a hydrogen reduction furnace with the temperature of 800 ℃ and the hydrogen flow of 2.0m3The reaction time was 8 hours, and ZTA/alloy steel mixed powder having a structure similar to that of example 1 was obtained.
(4) The ZTA/alloy steel mixed powder is filled into the honeycomb wall of a honeycomb-shaped die, the alloy steel powder is filled into the honeycomb holes of the honeycomb-shaped die, and the in-situ authigenic ZTA ceramic particle reinforced alloy steel base honeycomb-shaped macro-isomerism composite material can be obtained after rapid sintering (the sintering temperature is 1400 ℃ and the time is 2 hours), and the structure is similar to that of the embodiment 1.
The abrasion resistance of the in-situ authigenic ZTA ceramic particle reinforced alloy steel-based honeycomb-shaped macro-isomerism composite material prepared by the method is improved by 3.5 times compared with the traditional alloy steel.
Example 4
The embodiment relates to a preparation method of an in-situ synthesized ZTA ceramic particle reinforced high-chromium cast iron based honeycomb-shaped macro-isomerism composite material, which comprises the following specific steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate into deionized water, and then dripping citric acid to obtain a mixed solution, wherein the molar ratio of the aluminum nitrate nonahydrate to the zirconyl nitrate hydrate to the citric acid is 1:0.16: 0.13.
(2) Adjusting the pH value of the mixed solution to 2.5 by using nitric acid and ammonia water, adding 1.5 percent (mole fraction) of glycol serving as a dispersing agent into the mixed solution, fully stirring, and then putting into a constant-temperature water bath kettle to heat for 7 hours to obtain transparent sol with certain viscosity.
(3) Adding high-chromium cast iron powder with the particle size of 80 mu m into the sol, wherein the molar ratio of the high-chromium cast iron powder to the transparent sol is 0.7:1, quickly stirring for 0.3h until the high-chromium cast iron powder is completely solidified, then putting the high-chromium cast iron powder into a vacuum drying oven, wherein the temperature of the vacuum drying oven is 130 ℃, and the drying time is 11h to obtain ZTA/Fe2O3Mixing the powder, and putting the mixed powder into a hydrogen reduction furnace with the temperature of 650 ℃ and the hydrogen flow of 1.5m3And h, the time is 7h, and the ZTA/high-chromium cast iron mixed powder is obtained.
(4) The ZTA/high-chromium cast iron mixed powder is filled into the honeycomb wall of a honeycomb-shaped mold, the high-chromium cast iron powder is filled into the honeycomb holes of the honeycomb-shaped mold, and the in-situ self-generated ZTA ceramic particle reinforced high-chromium cast iron based honeycomb-shaped macro-isomerism composite material can be obtained after discharge plasma sintering (the sintering temperature is 1200 and the time is 4 hours), wherein the structure is similar to that of the embodiment 1.
The wear resistance of the in-situ synthesized ZTA ceramic particle reinforced high-chromium cast iron based honeycomb-shaped macro-isomerism composite material prepared by the method is improved by 4.5 times compared with the traditional high-chromium cast iron.
Claims (7)
1. A preparation method of an in-situ authigenic ZTA particle reinforced steel-based configuration composite material is characterized by comprising the following steps:
(1) dissolving aluminum nitrate nonahydrate and zirconyl nitrate hydrate in deionized water, dripping citric acid to obtain a mixed solution, adjusting the pH value of the mixed solution to be 1-3, adding ethylene glycol, fully stirring, and heating in a constant-temperature water bath kettle to obtain transparent sol;
(2) adding iron and steel-based powder into the transparent sol, rapidly stirring until the iron and steel-based powder is completely solidified, drying under a vacuum condition to obtain mixed powder of ZTA and iron and steel-based powder oxide, and reducing the mixed powder in a reducing furnace by reducing gas to obtain ZTA/iron and steel mixed powder;
(3) filling ZTA/steel mixed powder into the honeycomb wall of a honeycomb mould, filling steel-based powder into the honeycomb hole of the honeycomb mould, and pressing and sintering to obtain the in-situ self-generated ZTA particle reinforced steel-based configuration composite material;
the molar ratio of the aluminum nitrate nonahydrate to the zirconyl nitrate hydrate to the citric acid in the mixed solution obtained in the step (1) is 1 (0.1-0.3) to 0.1-0.26, and the molar percentage of the ethylene glycol added in the mixed solution after the pH value is adjusted is 0.5% -2.0%;
the molar ratio of the steel-based powder to the transparent sol in the step (2) is (0.3-0.7): 1.
2. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: and (1) jointly adjusting the pH value of the mixed solution by using nitric acid and ammonia water.
3. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: the heating conditions in the constant-temperature water bath kettle in the step (1) are as follows: heating for 6-10 h at 60-90 ℃.
4. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: the steel-iron-based powder in the step (2) is high-chromium cast iron, high-manganese steel or alloy steel powder, and the particle size of the powder is 20-100 mu m.
5. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: the drying conditions in the step (2) are as follows: drying the mixture for 10 to 16 hours in a vacuum drying oven at the temperature of between 100 and 140 ℃.
6. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: the reducing gas used in the reduction process in the step (2) is hydrogen, the temperature of the reducing furnace is 600-800 ℃, and the hydrogen flow is 1.0-2.0 m3The time is 5-8 h.
7. The method for preparing an in-situ self-generated ZTA particle reinforced steel-based configuration composite material according to claim 1, wherein the method comprises the following steps: the sintering temperature in the step (3) is 900-1400 ℃, and the time is 2-8 h.
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| AU2022224725A AU2022224725B2 (en) | 2021-08-31 | 2022-08-30 | Preparation method of in-situ synthesized zirconia toughened alumina (ZTA) ceramic particles-reinforced steel matrix structural composite |
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| CN114570482B (en) * | 2022-02-08 | 2023-05-09 | 徐州徐工矿业机械有限公司 | Three-liquid double-phase bimetal-ZTA ceramic composite material impact crusher plate hammer and manufacturing method thereof |
| CN114570481B (en) * | 2022-02-08 | 2023-05-05 | 徐州徐工矿业机械有限公司 | Impact crusher plate hammer made of high-chromium cast iron-based ZTA ceramic composite material and manufacturing method thereof |
| CN115627407B (en) * | 2022-10-19 | 2023-04-14 | 昆明理工大学 | Preparation method of ZTA ceramic reinforced iron-based composite material |
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| CN109706438A (en) * | 2018-12-28 | 2019-05-03 | 西安交通大学 | A kind of preparation method of the modified ZTA ceramic particle enhancing steel-based composite material in surface |
| CN111020360A (en) * | 2019-12-23 | 2020-04-17 | 昆明理工大学 | Non-infiltration type ceramic particle reinforced steel-based composite material and preparation method thereof |
| CN111809100A (en) * | 2020-07-17 | 2020-10-23 | 西安交通大学 | NiCrAlY high-temperature sintered ZTA particle reinforced steel-based composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114921708A (en) * | 2022-07-20 | 2022-08-19 | 昆明理工大学 | Preparation method of authigenic ZTA ceramic reinforced iron-based composite material |
| CN114921708B (en) * | 2022-07-20 | 2022-09-27 | 昆明理工大学 | Preparation method of authigenic ZTA ceramic reinforced iron-based composite material |
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| CN113862548A (en) | 2021-12-31 |
| AU2022224725B2 (en) | 2023-09-21 |
| AU2022224725A1 (en) | 2023-03-16 |
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