CN109095899B - Preparation method of alumina-based ceramic particle preform - Google Patents
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Abstract
The invention relates to a preparation method of an alumina-based ceramic particle preform, which comprises the steps of adding an inorganic binder into alumina ceramic particles, uniformly mixing, putting into an epoxy resin mold, pressing, putting into a microwave drying oven, and curing by microwave heating for 2-5 min; and stacking the solidified and demoulded prefabricated part in a sintering furnace, heating to 600-fold 850 ℃ under the protection of inert gas, preserving the heat for 1-2 hours, then cooling to 400 ℃, and cooling along with the furnace. According to the invention, microwave heating curing is adopted, so that the curing time is greatly shortened, the strength of the prefabricated body is not reduced, the production efficiency is greatly improved, and curing and demolding can be realized after heating without a large number of molds; the problem of adhesion of ceramic particles and a die is solved by adopting an epoxy resin die. The obtained prefabricated body is beneficial to infiltration of molten steel, eliminates the defect of pores of the prefabricated body, improves the high-temperature strength of the prefabricated body and avoids the defect of non-uniformity of ceramic particles.
Description
Technical Field
The invention relates to the field of preparation of metal-based wear-resistant materials, in particular to a preparation method of an alumina-based ceramic particle preform.
Background
In the industries of metallurgy, mine, electricity, building materials and the like, wear-resistant parts such as vertical grinding rollers, grinding discs, plate hammers, hammer heads and the like for crushing or grinding materials are developed from single wear-resistant metal materials to metal-based composite materials with high wear resistance. Because the nature of the reinforcing phase is greatly different from that of the metal matrix, the reinforcing phase prefabricated body is generally prepared firstly and then is compounded through different casting processes, and the preparation of the ceramic prefabricated body has great influence on the production of the final metal matrix composite material.
The patent (fransishabert 2003) discloses a method for making composite wear parts by adding an organic or inorganic binder to a ceramic preform followed by sintering, but does not specify the process for making the preform. The patent (Xian transportation university 2014) discloses a preparation method of an active element sintered ZTA particle reinforced steel-based composite grinding roller and a grinding disc. However, the method has the disadvantages that the price of metal powder is high, a graphite grinding tool is occupied in production, vacuum sintering is needed, and the efficiency of preparing a prefabricated body is low. The patent (Kunming technology university 2014) discloses a method for centrifugally casting a ceramic-metal composite vertical grinding roller, and a preform is prepared by adding a bonding agent into ceramic particles and an organic pore-forming agent. The ceramic preform is then preheated in a metal mold and centrifugally cast. The organic pore-forming agent is removed in the preheating stage, so that the strength of the prefabricated body is reduced, and the high-temperature molten steel in the subsequent centrifugal casting process is easy to cause the breakage of the prefabricated body and the agglomeration of ceramic particles, so that the ceramic particles of the final product are unevenly distributed. The patent (Qian soldier 2015) discloses a method for manufacturing a detachable ceramic alloy composite grinding roller, wherein a ceramic preform is prepared by uniformly mixing ceramic particles and low-melting-point alloy powder by using a bonding agent to obtain a mixture, filling the mixture into a mold cavity for molding, drying the mixture, putting the dried mixture into a vacuum furnace for sintering, and bonding the ceramic particles into the ceramic preform by using the low-melting-point alloy powder. The method needs metal powder for preparing the prefabricated body, so that the production cost is increased, in addition, vacuum sintering is needed, and the prefabricated body preparation efficiency is lower.
Disclosure of Invention
In order to overcome the problems, the invention provides a preparation method of an alumina-based ceramic particle preform, which adopts microwave heating curing, greatly shortens the curing time on the premise of not reducing the strength of the ceramic preform, greatly improves the production efficiency, and can realize curing and demolding after heating without a large number of molds; the problem of adhesion of ceramic particles and a die is solved by adopting an epoxy resin die. The obtained prefabricated body is beneficial to infiltration of molten steel, eliminates the defect of pores of the prefabricated body, improves the high-temperature strength of the prefabricated body and avoids the defect of non-uniformity of ceramic particles. In addition, during the subsequent sintering of the prefabricated body, the atmosphere protection method of a common sintering furnace is adopted, so that the problems that a vacuum sintering furnace is difficult to produce large pieces and has low efficiency due to the fact that a furnace chamber is small and the sintering period is long are solved.
The purpose of the invention and the technical problem to be solved are realized by adopting the following technical scheme. The preparation method of the alumina-based ceramic particle preform provided by the invention comprises the following steps:
(1) adding an inorganic binder into the alumina ceramic particles, uniformly mixing the ceramic particles and the inorganic binder, putting the mixture into an epoxy resin mold, pressing, putting the mixture of the ceramic particles and the inorganic binder and the epoxy resin mold into a microwave drying box, and curing the mixture by microwave heating for 2-5 min;
(2) removing the shell of the epoxy resin mold from the cured prefabricated part, ejecting the epoxy resin core part from the hole part of the prefabricated part by using special equipment, then placing the prefabricated part in an inert gas protection sintering furnace, heating to 600-plus 850 ℃ under the protection of inert gas, preserving heat for 1-2 hours, then cooling to 400 ℃, and cooling along with the furnace;
for the prefabricated part with larger size, the sintering temperature is 1200-1350 ℃, the temperature is kept for 30 minutes, then the temperature is reduced to 400 ℃, and the prefabricated part is cooled along with the furnace.
The purpose of the invention and the technical problem to be solved can be further realized by adopting the following technical scheme.
In the preparation method of the alumina-based ceramic particle preform, the microwave power in the step (1) is 3 kw.
In the preparation method of the alumina-based ceramic particle preform, the inorganic binder is added in the step (1) in an amount of 2-5% by weight of the alumina ceramic particles.
In the method for preparing the alumina-based ceramic particle preform, the inorganic binder is added in the step (1) in an amount of 3% by weight of the alumina ceramic particles.
In the preparation method of the alumina-based ceramic particle preform, the epoxy resin mold in the step (1) is made of epoxy resin material according to the shape of the preform.
In the preparation method of the alumina-based ceramic particle preform, the temperature in the step (2) is raised to 600-850 ℃ at a speed of 5-10 ℃/min, the temperature is kept for 1-2 hours, then the temperature is lowered to 400 ℃ at a speed of 2-5 ℃/min, and the alumina-based ceramic particle preform is cooled along with a furnace.
The preparation method of the alumina-based ceramic particle preform comprises the following steps of (1) heating the alumina-based ceramic particle preform to 750 ℃ at the speed of 6 ℃/min, preserving heat for 1.5 hours, then cooling the alumina-based ceramic particle preform to 400 ℃ at the speed of 5 ℃/min, and cooling the alumina-based ceramic particle preform along with a furnace.
In the preparation method of the alumina-based ceramic particle preform, the preform with a larger size has an area larger than 0.1m2The preform of (4).
In the preparation method of the alumina-based ceramic particle preform, the inorganic binder is composed of sodium silicate, silica sol and oxide powder, wherein the oxide powder is one or a mixture of more of aluminum oxide, magnesium oxide and nickel oxide, and the oxide powder is micron-sized or nano-sized; the mixing proportion of the sodium silicate, the silica sol and the oxide powder is 60-80 percent of the sodium silicate, 10-30 percent of the silica sol and 10-20 percent of the oxide powder by weight.
The preparation of the ceramic preform of the invention comprises 2 steps: pre-curing treatment and inert gas protection sintering. The pre-curing treatment means that the prefabricated body has certain wet strength and is convenient to carry. The curing mode adopts a microwave heating curing method, so that the demolding time is shortened from the traditional 30-60 minutes to 2-5 minutes, and the production efficiency is greatly improved. The inert gas protects sintering to carbonize organic components in the prefabricated part and remove crystal water of inorganic components, so that molten steel can be wetted in the later period, and the defect of pores in the composite material is avoided; the increase of the sintering temperature can sinter inorganic components in the adhesive, improve the high-temperature strength of the prefabricated part and resist the scouring of molten steel. By combining the two processes, a ceramic preform with certain normal-temperature and high-temperature strength can be prepared, and necessary conditions are provided for a molten steel infiltration process.
The microwave heating curing prefabricated part adopted by the invention has tensile strength similar to that of the common kiln type drying process, but the curing speed is 15-20 times of that of the common kiln type drying process, so that the rapid curing speed can bring three benefits: firstly, the production efficiency is greatly improved and the energy consumption is reduced; secondly, the curing and demoulding after heating can be realized without a large number of moulds; thirdly, the problem of adhesion of the ceramic particles and the die is solved by adopting an epoxy resin die under microwave. And the subsequent gas shielded sintering can carbonize organic matters in the adhesive and remove crystal water in the adhesive, thereby being beneficial to infiltration of molten steel and eliminating the defect of air holes. For large-scale casting parts, defects such as prefabricated part fracture, non-uniform ceramic particles and the like can be caused due to high-temperature molten steel erosion, and the high-temperature strength of the high-temperature sintered prefabricated part is improved, so that the defects can be avoided.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical means of the present invention more clearly understood, the present invention may be implemented in accordance with the content of the description, and in order to make the above and other objects, features, and advantages of the present invention more clearly understandable, the following specific preferred embodiments are described in detail.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to a method for preparing an alumina-based ceramic particle preform according to the present invention, and the specific implementation manner, features and effects thereof.
The invention comprises the following steps:
(1) adding an inorganic binder which accounts for 2-5% of the weight of the alumina ceramic particles into the alumina ceramic particles, uniformly mixing the ceramic particles and the inorganic binder, putting the mixture into an epoxy resin mold, putting the mixture of the ceramic particles and the inorganic binder and the epoxy resin mold into a microwave drying box after pressing, and heating the mixture by microwaves to cure the mixture, wherein the curing time is 2-5min, and the microwave power is 3 kilowatts; the inorganic binder consists of 60-80% of sodium silicate, 10-30% of silica sol and 10-20% of oxide powder by weight, wherein the oxide powder is one or a mixture of aluminum oxide, magnesium oxide and nickel oxide, and the oxide powder is micron-sized or nano-sized;
(2) removing the shell of the epoxy resin mold from the cured prefabricated part, ejecting the epoxy resin core part from the hole part of the prefabricated part by using special equipment, stacking the cured and demolded prefabricated part in a sintering furnace, introducing inert protective gas nitrogen or argon, heating to 600 plus materials at the speed of 5-10 ℃/min, preserving heat for 1-2 hours, then cooling to 400 ℃ at the speed of 2-5 ℃/min, and cooling along with the furnace;
for larger sizes (e.g. greater than 0.1m area)2The prefabricated member) is heated to 1200-1350 ℃ at the speed of 5-10 ℃/min, is kept warm for 30 minutes, is cooled to 400 ℃ at the speed of 2-5 ℃/min, and is cooled along with the furnace.
Example 1:
adding 3% of adhesive (the adhesive is composed of 60% of sodium silicate, 20% of silica sol and 20% of mixed powder of nano-scale or micro-scale alumina and nickel oxide) into the alumina-based ceramic particles, uniformly mixing, filling the mixture into an epoxy resin grinding tool, pressing, putting into a microwave drying oven, drying and curing for 3 minutes under the microwave power of 3 kilowatts, and testing the tensile strength of the cured and demoulded prefabricated part to be 1.4 Mpa.
Removing the shell of an epoxy resin mold from the cured prefabricated part, ejecting the core part of the epoxy resin from the porous part of the prefabricated part by using special equipment, then putting the cured and demolded prefabricated part into a sintering furnace, introducing inert protective gas nitrogen, heating to 750 ℃ at 6 ℃/min, preserving heat for 1.5 hours, then cooling to 400 ℃ at 5 ℃/min, and furnace-cooling to obtain an alumina-based ceramic particle prefabricated part, wherein the tensile strength of the prefabricated part is not changed from the tensile strength after curing and demolded. And placing the prepared alumina-based ceramic particle preform into a casting grinding tool, and casting to obtain the metal-based composite material.
Example 2:
adding 3% of adhesive (the adhesive is composed of 60% of sodium silicate, 20% of silica sol and 20% of mixed powder of nano-scale or micro-scale alumina and magnesium oxide) into the alumina-based ceramic particles, uniformly mixing, filling the mixture into an epoxy resin grinding tool, pressing, putting into a microwave drying oven, drying and curing for 3 minutes under the microwave power of 3 kilowatts, and testing the tensile strength of the cured and demoulded prefabricated part to be 1.5 Mpa.
Removing the shell of an epoxy resin mold from the cured prefabricated part, ejecting the epoxy resin core part of the porous part of the prefabricated part by using special equipment, then putting the cured and demolded prefabricated part into a sintering furnace, introducing inert protective gas nitrogen, heating to 1250 ℃ at 6 ℃/min, preserving heat for 0.5 hour, then cooling to 400 ℃ at 5 ℃/min, and furnace-cooling to obtain an alumina-based ceramic particle prefabricated part, wherein the tensile strength of the prefabricated part is not changed from the tensile strength after curing and demolding, and a new binding phase is formed after the melting point (1089 ℃) of sodium silicate is shown. And placing the prepared alumina-based ceramic particle preform into a casting grinding tool, and casting to obtain the metal-based composite material.
Example 3:
adding 2% of adhesive (the adhesive is composed of 60% of sodium silicate, 20% of silica sol and 20% of nano-scale or micron-scale nickel oxide powder) into the alumina-based ceramic particles, uniformly mixing, filling the mixture into an epoxy resin grinding tool, pressing, putting into a microwave drying oven, drying and curing for 3 minutes under the microwave power of 3 kilowatts, and testing the tensile strength of the cured and demoulded prefabricated part to be 1.2 Mpa.
Removing the shell of an epoxy resin mold from the cured prefabricated part, ejecting the core part of the epoxy resin from the porous part of the prefabricated part by using special equipment, then putting the cured and demolded prefabricated part into a sintering furnace, introducing inert protective gas nitrogen, heating to 800 ℃ at the speed of 8 ℃/min, preserving heat for 1.5 hours, then cooling to 400 ℃ at the speed of 5 ℃/min, and furnace-cooling to obtain an alumina-based ceramic particle prefabricated part, wherein the tensile strength of the prefabricated part is not changed from the tensile strength after curing and demolded. And placing the prepared alumina-based ceramic particle preform into a casting grinding tool, and casting to obtain the metal-based composite material.
Example 4:
adding 4% of adhesive (the adhesive is composed of 60% of sodium silicate, 20% of silica sol and 20% of nano-scale or micron-scale magnesium oxide powder) into the alumina-based ceramic particles, uniformly mixing, filling the mixture into an epoxy resin grinding tool, pressing, putting into a microwave drying oven, drying and curing for 3 minutes under the microwave power of 3 kilowatts, and testing the tensile strength of the cured and demoulded prefabricated part to be 1.3 Mpa.
Removing the shell of the epoxy resin mold from the cured prefabricated part, ejecting the epoxy resin core part of the porous part of the prefabricated part by using special equipment, then putting the cured and demolded prefabricated part into a sintering furnace, introducing inert protective gas nitrogen, heating to 850 ℃ at 8 ℃/min, preserving heat for 1.3 hours, then cooling to 400 ℃ at 5 ℃/min, and furnace-cooling to obtain the alumina-based ceramic particle prefabricated part, wherein the tensile strength of the prefabricated part is not changed from the tensile strength after curing and demolded. And placing the prepared alumina-based ceramic particle preform into a casting grinding tool, and casting to obtain the metal-based composite material.
The inventors also examined the tensile strength of preforms obtained with different binder addition at different microwave curing times, and the results are given in table 1 below:
TABLE 1 tensile Strength of preforms obtained at different microwave curing times
As can be seen from the above table, when the microwave curing time is 180s, i.e. 3 minutes, the tensile strength of the obtained preform is relatively large, and the optimum amount of the binder to be added is 3%. However, the results obtained with binder additions of 2% or 4% do not differ much from those obtained with 3%.
According to the invention, on the premise of not reducing the tensile strength of the prefabricated member, the demolding time of the prefabricated member is greatly shortened from the traditional 30-60 minutes to 2-5 minutes, so that the production efficiency is greatly improved. A large number of moulds are not needed, and the problem of adhesion of the ceramic particles and the moulds is solved.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical essence of the present invention by those skilled in the art can be made within the technical scope of the present invention without departing from the technical scope of the present invention.
Claims (4)
1. A method for preparing an alumina-based ceramic particle preform is characterized by comprising the following steps:
(1) adding an inorganic binder which accounts for 2-5% of the weight of the alumina ceramic particles into the alumina ceramic particles, uniformly mixing the ceramic particles and the inorganic binder, putting the mixture into an epoxy resin mold, putting the mixture of the ceramic particles and the inorganic binder and the epoxy resin mold into a microwave drying box after pressing, and heating by microwaves to cure the mixture, wherein the microwave power is 3 kilowatts, and the curing time is 3 min;
the inorganic binder consists of 60-80% of sodium silicate, 10-30% of silica sol and 10-20% of oxide powder by weight; wherein, the oxide powder is one or a mixture of more of aluminum oxide, magnesium oxide and nickel oxide, and the oxide powder is micron-sized or nano-sized;
(2) removing the shell of the epoxy resin mold from the cured prefabricated part, ejecting the epoxy resin core part from the hole part of the prefabricated part by using special equipment, then placing the prefabricated part in an inert gas protection sintering furnace, heating to 600-850 ℃ at the speed of 5-10 ℃/min under the protection of inert gas, preserving heat for 1-2 hours, then cooling to 400 ℃ at the speed of 2-5 ℃/min, and furnace-cooling.
2. The method for producing an alumina-based ceramic particle preform according to claim 1, wherein the inorganic binder is added in an amount of 3% by weight of the alumina ceramic particles in the step (1).
3. The method for preparing an alumina-based ceramic particle preform according to claim 1, wherein the epoxy resin mold of the step (1) is a corresponding mold made of an epoxy resin material according to the shape of the preform.
4. The method for preparing an alumina-based ceramic particle preform according to claim 1, wherein the temperature in the step (2) is raised to 750 ℃ at a rate of 6 ℃/min, and the temperature is maintained for 1.5 hours, and then the temperature is lowered to 400 ℃ at a rate of 5 ℃/min, and the preform is furnace-cooled.
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