CN109049267B - Ti-Fe micro powder coated multi-channel ceramic preform and preparation method and application thereof - Google Patents
Ti-Fe micro powder coated multi-channel ceramic preform and preparation method and application thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B28B1/00—Producing shaped prefabricated articles from the material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention belongs to the field of material processing, and discloses a multi-channel ceramic preform coated with Ti-Fe micro powder, and a preparation method and application thereof. According to the invention, the alloy powder is obtained near the deep eutectic point of the Fe-Ti alloy by a Mechanical Alloying (MA) method, the melting temperature of the alloy powder can reach 1085 ℃, the alloy powder and ZTA ceramic particles are subjected to heat preservation at 1250-1550 ℃ by a pressureless sintering method, molten liquid Ti is promoted to perform activation treatment on the ZTA surface, the ZTA and surface activation effects can be obviously improved, a Ti-O transition layer is formed between the ceramic and the binder, so that the crushing strength of the preform is improved, the wettability of the ceramic surface and a steel solution is improved, and the crushing strength of the preform can reach 5 MPa.
Description
Technical Field
The invention belongs to the field of material processing, and particularly relates to a multi-channel ceramic preform coated with Ti-Fe micro powder, and a preparation method and application thereof.
Background
The ceramic particles in the particle reinforced steel-based composite material play a role in improving the wear resistance of the steel material. In the service process, the steel matrix supports the ceramic particles, so that the ceramic particles protrude out of the steel matrix along with the increase of the abrasion loss of the steel matrix, and further abrasion of steel materials is prevented. The bonding and forming of the ceramic particles and the interface bonding strength between the ceramic particles and the metal are the key points for improving the performance of the composite material in the process of preparing the composite material.
In the field of material processing, zirconia toughened alumina ceramics (ZTA) have been widely introduced as fillers in high chromium cast iron, steel, high manganese steel, and partially cemented carbide, because of their excellent toughness and hardness. Moreover, the method has better economic applicability and is also beneficial to large-scale and batch production of materials; in particular, in the aspects of friction reduction and wear resistance of materials, ZTA particles are often used as a wear-resistant reinforcing phase of a metal material to improve the impact wear resistance of the material. In addition, in the steel smelting process, the ZTA ceramic micro powder with micro-nano scale is frequently used as an inoculant, the effect of refining grains is achieved, and the purpose of improving the overall mechanical property of the material is achieved. However, the ZTA ceramic has the characteristics of good interface stability, difficult molding, extremely low wettability with steel melt, and the like, and becomes a major bottleneck for the development of steel-based ceramic composite materials.
The combination mode of the ceramic particles and the intermetallic interface determines the combination strength of the formed interface, at present, the ceramic particles and the intermetallic interface are mainly combined mechanically, and the metallurgical combination is difficult, which is mainly due to the characteristics of different chemical properties, thermal expansion coefficients and the like of the ceramic and the metal, so that the poor combination of the ceramic particles and the intermetallic interface is caused. In addition, the ZTA ceramic preform is mainly prepared by a process combining Mechanical Alloying (MA) and pressureless sintering. The MA process utilizes the long-time violent impact and collision between powder particles and grinding balls to promote the full atomic diffusion among the powder, and the pressureless sintering mainly generates atomic diffusion between activated powder and the surface of ceramic, and in addition, the ceramic particles can be connected and formed with certain strength through the sintering of the powder. The powder which can generate diffusion reaction with the ceramic surface promotes the ceramic surface to have certain metallicity, can obviously improve the wettability of the ceramic surface in molten metal, and realizes full contact between the ceramic surface and a metal solution in the subsequent casting and infiltrating process. Therefore, there is a need to develop a ceramic that can be metallurgically bonded to the intermetallic interface.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention mainly aims to provide a preparation method of a multi-channel ceramic preform coated by Ti-Fe micro powder. According to the method, the Fe-Ti mixed powder is subjected to alloying treatment, the Ti content is controlled within the range of 25-35 wt%, the powder and the ceramic are mixed and sintered, the high bonding strength among ceramic particles can be realized, the crushing strength of the prefabricated body can reach 5MPa, and the added Ti powder is combined with O in ZTA ceramic to form an effective activation effect on the surface of the ceramic.
The invention also aims to provide the multi-channel ceramic preform coated with the Ti-Fe micro powder prepared by the method.
The invention further aims to provide application of the multi-channel ceramic preform coated by the Ti-Fe micro powder in preparation of high-chromium cast iron-based or high-manganese steel-based composite materials and the like.
The purpose of the invention is realized by the following scheme:
a preparation method of a multi-channel ceramic preform coated by Ti-Fe micro powder mainly comprises the following steps:
(1) mixing powder and alloying: mixing reduced iron powder and Ti powder, and adding the mixture into a ball milling tank for ball milling to alloy, thereby obtaining a mixed powder binder;
(2) mixing materials: mixing the mixed powder binder obtained in the step (1) with ZTA particles, adding water glass as a curing agent and paraffin particles as a pore-forming agent, and stirring to uniformly coat the powder binder on the surfaces of the ZTA ceramic particles to obtain a mixed material;
(3) and (3) curing: filling the mixed material obtained in the step (2) into a forming die, shaping and compacting the prefabricated body by a fastening grinding tool, and continuously introducing CO2Curing the gas, drying and demoulding to obtain a cured and molded prefabricated body;
(4) vacuum pressureless sintering: and (4) putting the preform solidified and formed in the step (3) into a vacuum sintering furnace for sintering to obtain the ceramic preform with certain strength and porosity.
In order to prevent the specific surface area of the mixed powder after ball milling from increasing and the mixed powder is easy to react with oxygen in the air, the step (1) and the step (2) are generally carried out under protective gas, and the protective gas can be one of argon or nitrogen;
the purity of the reduced iron powder in the step (1) is 99.99%, and the granularity is less than or equal to 100 meshes; the purity of Ti powder is 99.99 percent, and the granularity is less than or equal to 300 meshes;
the using amount of the reduced iron powder and the Ti powder in the step (1) is controlled to be close to the components of the Ti-Fe eutectic area, and preferably the Ti powder accounts for 25-35 wt% of the total mass of the reduced iron powder and the Ti powder;
the ball mill in the step (1) is preferably a planetary ball mill, and the ball milling process comprises the following steps: the ball milling time is 24-30 h, the diameter of the grinding ball is 5-10 mm, the weight ratio of the grinding ball to the mixed powder is 10:1, and the rotating speed of the ball mill is 300-450 r/min.
The particle size of the ZTA ceramic particles in the step (2) is 8-10 meshes; the particle size of the paraffin particles in the step (2) is 10-12 meshes;
the using amount of the mixed powder in the step (2) is 3-8 wt% of the total weight of the mixed material obtained in the step (2); water glass (Na) described in step (2)2SiO3·9H2O) is 3-7% of the weight of the alloy powder in the step (2), preferably 5%; the dosage of the paraffin particles in the step (2) is 1-3 wt% of the total weight of the mixed material obtained in the step (2); the balance of ZTA particles;
the stirring in the step (2) is to uniformly mix the raw materials, and the purpose of the step can be realized at the rotating speed which is conventionally used in the field, so that the stirring speed is not limited, and the stirring is preferably performed for 5-15 min by using a glass rod;
the forming die in the step (3) is preferably a hollow cube with the thickness of 30mm × 20mm, 20mm × 10mm and 10mm in the middle, the die is made of wood fiber materials, and the wood fiber materials are connected with the sectional modules through fastening bolts.
And (3) fastening is to enable the mixed material placed in the mold to pass through a center line of the mold to be centered and jointed, and then fastening bolts.
Continuously introducing CO in the step (3)2The method is characterized in that a forming die filled with a mixture is placed in a container with an open air outlet, and the aeration rate is 40-60 cm3And/s, the inflation time is 0.5-1 h, the pipe diameter of the air inlet pipe is 55-59 mm, and the pipe diameter of the air outlet hole is larger than that of the air inlet hole but smaller than 100 mm.
The drying in the step (3) is to keep the temperature in a vacuum drying oven at 60-80 ℃ for 1-2 h;
the sintering in the step (4) means that the vacuum degree in the sintering process is kept at 2.9 × 10-3Pa, controlling the sintering heat preservation temperature at 1250-1550 ℃, preserving the heat for 1h, and cooling to room temperature along with the furnace.
The multi-channel ceramic preform coated by the Ti-Fe micro powder prepared by the method.
The multi-channel ceramic preform coated by the Ti-Fe micro powder is applied to the preparation of high-chromium cast iron-based or high-manganese steel-based composite materials and the like.
The mechanism of the invention is as follows:
ti and O have good bonding characteristics, but the melting point of pure Ti is 1670 ℃, which is far higher than the melting temperature of steel materials, which is not beneficial to bonding with oxygen in ZTA, and the activation effect on the ZTA surface is reduced.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the Fe-Ti micro powder as a binding agent of the ceramic particles can form diffusion reaction with atoms on the surface of the ceramic, so that the reaction characteristic of the surface of the ceramic can be greatly improved, and the strength and the forming capability of the preform are improved.
(2) In the shaping and curing process of the prefabricated body, the curing agent and CO2The method is suitable for preparing the metal matrix composite material with higher requirement on the forming capacity of the preform, and can obviously improve the forming efficiency of the preform and the complex profileThe molding ability of (1).
(3) The addition of the paraffin particles can improve the void forming capability of the preform, increase the cellular porous characteristic of the preform and improve the infiltration capability of ZTA ceramics.
Drawings
FIG. 1 is a photograph of a multi-channel ceramic preform coated with Ti-Fe fine powder prepared in example 1;
FIG. 2 is a back-scattered image of the ceramic particles and binder in the sintered preform and an EDS line scan of the transition layer of example 1.
FIG. 3 is a wetting angle measurement of the surface of ZTA ceramic after sintering in example 1 with high chromium cast iron.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference. The ball mill used in the examples was a YXQM planetary ball mill.
The porosity of the preform is obtained by testing with an Archimedes drainage method, and the specific calculation steps are as follows: the pores of the ceramic preform are open pores, the volume percentage of the pores in the entire material is measured by an Archimedes method, and the porosity is represented by P. The porosity of the preform was determined in the test by a water boiling method. First, the required dry weight of the sample is weighed as m0(ii) a The weighed sample is placed in a clean beaker, and distilled water is injected into the beaker until the sample is submerged. And then placing the beaker on an electric furnace, heating to boil, and keeping the boiling state for 1-2h to ensure that the distilled water completely permeates into the gaps of the preform. The heating was then stopped and allowed to cool to room temperature. Then the sample is quickly taken out and put into a balance tray which is prepared for weighing in advance, and the suspended weight m of the saturated sample in water is weighed1(ii) a Taking out the saturated sample, wiping off water on the surface of the saturated sample, and quickly weighing the mass m of the saturated sample2The porosity P is calculated by a formula.
P＝(m2-m0)/(m2-m1)
The crush strength of the preform was tested by the following procedure: the prepared hollow cylindrical ZTA ceramic preform was placed between two flat plates of a testing machine so that the axis of the sample was parallel to the flat plates. Continuously loading without vibration, wherein the loading speed is between 0.5MPa/s and 3MPa/s, the loading time is 10s, and the crushing strength is according to the formula:
K＝F(D-e)/Le2
in the formula: k-radial crush strength in Mega pascals (MPa);
f- -crushing load in cattle (N);
l-sample length in millimeters (mm);
d is the outer diameter of the sample in millimeters (mm);
e-sample wall thickness in millimeters (mm).
Example 1:
(1) mixing the reduced Fe powder with the purity of 99.99 percent and the granularity of 100-200 meshes and the Ti powder with the purity of 99.99 percent and the granularity of 300 meshes according to the proportion that the Ti powder accounts for 30 wt.% of the total weight of the Ti powder and the iron powder, and then adding the mixed powder into a ball milling tank for ball milling alloying, wherein the ball milling process comprises the following steps: the ball-material ratio is 10:1, the rotating speed is 300r/min, and the ball milling time is 24h, so that the Fe powder and the Ti powder are uniformly mixed to obtain the powder binder.
The granularity of the mixed powder after ball milling is reduced, the surface energy is rapidly increased, and the powder is easy to react with oxygen in the air, so that the powder needs to be taken out from a glove box filled with inert gas;
(2) selecting ZTA ceramic particles (ZrO) with the particle size of 8-10 meshes in a die consisting of a 30mm × 20mm, × 10mm hollow cube and a phi 10mm cylinder in the middle220 wt.%, Al2O380 wt.%), Ti-Fe mixed micropowder 2.4g, water glass 0.12g, paraffin particles of 10-12 meshes as pore-forming agent 0.65 g. Stirring with glass rod for 10min to coat the binder on ZTA particle surface, wherein the whole process is N2The method is carried out in a protective atmosphere.
(3) Placing the preform in a glove box, opening the air outlet, and introducing CO2Gas is introduced for 0.5h at an inflation rate of 50cm3S, to be predictedAnd (3) after the solidification and the forming of the prepared body, placing the mold into a constant temperature furnace at 60 ℃, preserving heat for 30min, drying, and demoulding and taking out the prefabricated body.
(4) The vacuum degree of the sintering process of the preform prepared by pressureless sintering is kept at 2.9 × 10-3Pa, the sintering heat preservation temperature is 1300 ℃, the heat preservation time is 1h, and the multi-channel ZTA ceramic preform with the activated surface is prepared after the temperature is cooled to the room temperature along with the furnace.
FIG. 1 is a photograph of the ZTA ceramic preform obtained in the example.
FIG. 2 is a back-scattered image of ceramic particles and binder in the sintered preform and an EDS line scan of the transition layer in example 1. from FIG. 2, it can be seen that oxygen in ZTA ceramic and Ti in powder binder are the main components for forming the transition layer, and Ti reacts with O in ZTA ceramic to form oxide, which generates oxygen-deprived regions on the ceramic surface, and these regions form effective activation; a Ti-O transition layer of 2-8 um is formed between the ceramic and the binder, the bonding strength between the ceramic particles is high, no obvious cracking phenomenon is found, the porosity of the prefabricated body is 60%, and the crushing strength is 5 MPa.
Fig. 3 is a measurement result of the wetting angle between the sintered ZTA surface and the metallic high-chromium cast iron in example 1, and it can be seen that the wetting angle is less than 15.1 °, and the ceramic surface shows a good wetting effect, which indicates that the sintered ZTA ceramic surface can be well wetted by the wear-resistant molten steel, and effective bonding or element diffusion can be formed at the composite interface, which is beneficial to the formation of the metallurgical interface.
Example 2
(1) Putting the ball milling tank into a glove box, introducing inert gas, mixing reduced Fe powder with the purity of 99.99 percent and the granularity of 100 plus materials of 200 meshes with Ti powder with the purity of 99.99 percent and the granularity of 300 meshes according to the weight ratio of the Ti powder to the iron powder of 25 percent; and (3) tightly sealing the ball milling tank, and carrying out alloying treatment in a YXQM planetary ball mill, wherein the ball diameter of a milling ball is 10mm, the ball-material ratio is 10:1, the rotating speed is 300r/min, and the ball milling time is 24h, so that the Fe and Ti powder can fully react to obtain the powder binder.
Because the granularity of the mixed powder after ball milling is reduced, the surface energy is rapidly increased, and the powder is very easy to react with oxygen in the air, the ball milling tank is still put into a glove box filled with inert gas for tank opening and powder taking, and the taken alloy powder is put into a closed container for storage;
(2) selecting ZTA ceramic particles (ZrO) with the particle size of 8-10 meshes in a die consisting of a 30mm × 20mm, × 10mm hollow cube and a phi 10mm cylinder in the middle220 wt.%, Al2O380 wt.%), Ti-Fe mixed micropowder 2.4g, water glass 0.12g, paraffin particles of 10-12 meshes as pore-forming agent 0.65 g. Stirring with glass rod for 10min until the surface of ZTA particles is coated with binder uniformly, and the whole process is N2The method is carried out in a protective atmosphere.
(3) Placing the preform in a glove box, opening the air outlet, and introducing CO2The gas is introduced for 0.5h at an inflation rate of 50cm3And/s, after the prefabricated body is solidified and formed, placing the mould into a constant temperature furnace at 60 ℃, preserving heat for 30min, drying, and demoulding and taking out the prefabricated body.
(4) The prefabricated body is prepared by pressureless sintering, and the vacuum degree in the sintering process is kept at 2.9 × 10-3Pa, the sintering temperature is 1250 ℃, the heat preservation time is 1h, and the multi-channel ZTA ceramic preform with the activated surface is prepared after the temperature is cooled to the room temperature along with the furnace.
According to the obtained ZTA ceramic preform, a back scattering image of ceramic particles and a binder in the sintered preform and an EDS line scanning chart of a transition layer can be judged, a Ti-O transition layer of about 1-3 um is formed between the ceramic particles and the binder, the porosity of the preform is 62%, and the crushing strength is 1 MPa.
The wetting angle between the sintered ZTA surface and the metallic high-chromium cast iron in the embodiment 2 is also smaller than 15.1 degrees, which shows that the sintered ZTA ceramic surface of the embodiment can be well wetted by the wear-resistant molten steel, and can form effective combination or element diffusion on a composite interface, thereby being beneficial to the formation of a metallurgical interface.
Example 3:
(1) taking Ti powder with the purity of 99.99 percent and the granularity of 100-200 meshes, reducing Fe powder and Ti powder with the purity of 99.99 percent and the granularity of 300 meshes, mixing the powder according to 35 wt.% of the Ti powder and the iron powder, and then adding the powder into a ball milling tank for ball milling alloying, wherein the ball milling process comprises the following steps: the ball-material ratio is 10:1, the rotating speed is 300r/min, and the ball milling time is 24h, so that the Fe powder and the Ti powder are uniformly mixed to obtain the powder binder.
The granularity of the mixed powder after ball milling is reduced, the surface energy is rapidly increased, and the powder is easy to react with oxygen in the air, so that the powder needs to be taken out from a glove box filled with inert gas;
(2) selecting ZTA ceramic particles (ZrO) with the particle size of 8-10 meshes in a die consisting of a 30mm × 20mm, × 10mm hollow cube and a phi 10mm cylinder in the middle220 wt.%, Al2O380 wt.%), Ti-Fe mixed micropowder 2.4g, water glass 0.12g, paraffin particles of 10-12 meshes as pore-forming agent 0.65 g. Stirring with glass rod for 10min until the surface of ZTA particles is coated with binder uniformly, and the whole process is N2The method is carried out in a protective atmosphere.
(3) Placing the preform in a glove box, opening the air outlet, and introducing CO2The gas is introduced for 0.5h at an inflation rate of 50cm3And/s, after the prefabricated body is solidified and formed, placing the mould into a constant temperature furnace at 60 ℃, preserving heat for 30min, drying, and demoulding and taking out the prefabricated body.
(4) The prefabricated body is prepared by pressureless sintering, and the vacuum degree in the sintering process is kept at 2.9 × 10-3Pa, the sintering heat preservation temperature is 1300 ℃, the heat preservation time is 1h, and the multi-channel ZTA ceramic preform with the activated surface is prepared after the temperature is cooled to the room temperature along with the furnace.
According to the obtained ZTA ceramic preform, a backscattering image of ceramic particles and a binder in the sintered preform and an EDS line scanning image of a transition layer can be determined, a 2-5 um Ti-O transition layer is formed between the ceramic and the binder, the bonding strength between the ceramic particles is high, no obvious cracking phenomenon is found, the porosity of the preform is 61%, and the crushing strength is 5 MPa.
The wetting angle between the sintered ZTA surface and the metallic high-chromium cast iron in the embodiment 3 is also smaller than 15.1 degrees, which shows that the sintered ZTA ceramic surface of the embodiment can be well wetted by the wear-resistant molten steel, and can form effective combination or element diffusion on a composite interface, thereby being beneficial to the formation of a metallurgical interface.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. A preparation method of a multi-channel ceramic preform coated by Ti-Fe micro powder is characterized by mainly comprising the following steps:
(1) mixing powder and alloying: mixing reduced iron powder and Ti powder, and adding the mixture into a ball milling tank for ball milling to alloy, thereby obtaining a mixed powder binder;
(2) mixing materials: mixing the mixed powder binder obtained in the step (1) with ZTA particles, adding water glass as a curing agent and paraffin particles as a pore-forming agent, and stirring to uniformly coat the powder binder on the surfaces of the ZTA ceramic particles to obtain a mixed material;
(3) and (3) curing: filling the mixed material obtained in the step (2) into a forming die, shaping and compacting the prefabricated body by a fastening grinding tool, and continuously introducing CO2Curing the gas, drying and demoulding to obtain a cured and molded prefabricated body;
(4) vacuum pressureless sintering: placing the prefabricated body after being cured and molded in the step (3) into a vacuum sintering furnace for sintering to obtain a ceramic prefabricated body with certain strength and porosity;
the amount of the reduced iron powder and the Ti powder in the step (1) is 25-35 wt% of the total mass of the reduced iron powder and the Ti powder;
the ball milling process in the step (1) comprises the following steps: the ball milling time is 24-30 h, the diameter of the grinding ball is 5-10 mm, the weight ratio of the grinding ball to the mixed powder is 10:1, and the rotating speed of the ball mill is 300-450 r/min.
2. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
and (3) performing the step (1) and the step (2) under protective gas, wherein the protective gas is one of nitrogen or argon.
3. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the purity of the reduced iron powder in the step (1) is 99.99%, and the granularity is less than or equal to 100 meshes; the purity of Ti powder is 99.99%, and the granularity is less than or equal to 300 meshes.
4. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the using amount of the mixed powder in the step (2) is 3-8 wt% of the total weight of the mixed material obtained in the step (2); the amount of the water glass in the step (2) is 3-7% of the weight of the alloy powder in the step (2); the dosage of the paraffin particles in the step (2) is 1-3 wt% of the total weight of the mixed material obtained in the step (2); the balance of ZTA particles.
5. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the fastening in the step (3) is to center and joint the mixed material placed in the mold through the center line of the mold, and then fasten bolts;
continuously introducing CO in the step (3)2The gas means that a mould containing the mixed material is placed in a container with an open air outlet, and the aeration rate is 40-60 cm3The inflation time is 0.5-1 h, the pipe diameter of the air inlet pipe is 55-59 mm, and the pipe diameter of the air outlet hole is larger than that of the air inlet hole but smaller than 100 mm;
and (3) drying refers to keeping the temperature in a vacuum drying oven at 60-80 ℃ for 1-2 h.
6. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the sintering in the step (4) is firingThe vacuum degree in the process of forming is kept at 2.9 × 10-3Pa, controlling the sintering heat preservation temperature at 1250-1550 ℃, preserving the heat for 1h, and cooling to room temperature along with the furnace.
7. A Ti-Fe micropowder-coated multi-channel ceramic preform prepared according to the method of any one of claims 1 to 6.
8. The use of the Ti-Fe micropowder-coated multi-channel ceramic preform of claim 7 in the preparation of steel-based composites.
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