Method for manufacturing iron-based ceramic composite reinforced wear-resistant material by vacuum impregnation method and preparation method thereof

Abstract

The present invention relates to the technical field of iron-based ceramic composite materials, and specifically relates to a method for manufacturing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration and its preparation method, which includes the following steps: mixing ceramic particles with a particle size of 0.8 - 2.2 mm with a binder, an activator, and paraffin particles in proportion and stirring to form a mixture; placing the stirred mixture in a mold of a ceramic preform for molding under pressure, and then putting the mold into a resistance furnace. The iron-based ceramic composite reinforced wear-resistant material of the present invention is formed by mixing ceramic particles with a binder, an activator, and paraffin particles in proportion, molding under pressure, and then sintering in a resistance furnace to form a ceramic preform with a porous structure. Through vacuum pumping of high-temperature iron-based alloy liquid and infiltration into the pores of the ceramic preform, the formed composite reinforced wear-resistant material has a coordinated improvement in strength, toughness, and wear resistance.

Description

Technical Field

[0001] The present invention relates to the technical field of iron-based ceramic composite materials, and particularly to a method for manufacturing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration and its preparation method. Background Art

[0002] The application and research of wear-resistant materials play an important role in the current industrial development. For example, mechanical equipment in the cement, machinery, electric power, mining, metallurgy, shipbuilding, chemical and coal industries, grinding balls, grinding discs, grinding rollers and accessories of various mills, and also the crushing walls, crushing plates, and hammer plates of impact crushers.

[0003] It is difficult to balance and coordinate the improvement of the strength, toughness and wear resistance of existing iron-based ceramic materials. The balanced improvement of performance is the technical difficulty of the present invention. At the same time, the corrosion resistance and thermal shock stability of the product are poor, which further limits the use efficiency of the product. Based on this, the present invention makes further improvement treatment. Summary of the Invention

[0004] Aiming at the defects of the existing technology: 1. Forcibly discharging the air in the pores of the ceramic preform during the infiltration of the iron-based alloy liquid solves the problem of difficult natural discharge. 2. The infiltration kinetic energy of the iron-based alloy liquid is enhanced by the pressure formed by vacuum negative pressure, thereby improving the bonding strength of the composite material. 3. The molten iron composition is purified in a negative pressure environment to improve the purity of the molten iron of the iron-based alloy. The purpose of the present invention is to provide a method for manufacturing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration and its preparation method to solve the problems raised in the above background art.

[0005] The present invention solves the technical problems by adopting the following technical solutions:

[0006] The present invention provides a preparation method for manufacturing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration, including the following steps:

[0007] Step 1: Mix ceramic particles with a particle size of 0.8 - 2.2 mm, a binder, an activator, and paraffin particles in proportion and stir to form a mixture;

[0008] Step 2: Place the mixture after stirring in Step 1 in a mold of a ceramic preform, press it into shape, then put the mold into a resistance furnace, heat it to 120 °C, demold after 2 hours, and then sinter it at a high temperature of 1250 °C for 12 hours to cause a phase change, and naturally cool it to room temperature to obtain a ceramic preform with a multi-porous structure;

[0009] Step 3: Place the ceramic preform in a formed film shell, preheat it to 450 - 850 °C, and then place the preheated film shell in a vacuum furnace;

[0010] Step 4: heating the iron-based alloy to 1520-1550° C., melting to form a high-temperature iron-based alloy liquid, and pouring it into the membrane shell of the vacuum furnace, closing the sealing cover of the vacuum furnace to keep it in a closed state, and starting the vacuum pump to evacuate the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic prefabricated block is evacuated, thereby allowing the iron-based alloy liquid to infiltrate the pores of the ceramic prefabricated body, keeping the temperature for 16-24 hours, and then cooling to room temperature to obtain the composite reinforced wear-resistant material of the present invention;

[0011] The iron-based alloy comprises the following raw materials in parts by weight: 2-3.5 parts of C, 10-30 parts of Cr, 70-75 parts of Fe, 1.5-2 parts of Mo, and 1.5-2 parts of V.

[0012] Preferably, the ratio of the ceramic particles to the binder, the activator, and the paraffin particles is (8-11):(2-3):(1-3):1; wherein the activator is one of aluminum powder, silicon carbide powder, and tungsten carbide powder; and the binder is an inorganic binder;

[0013] The porosity of the ceramic prefabricated block with a porous structure is 35-60%; the membrane shell preheated for molding is made of metal heat-resistant steel.

[0014] Preferably, the composite reinforced wear-resistant material further comprises 8-13 parts of a reinforcing agent; the reinforcing agent is used for reinforcing and improving the iron-based alloy;

[0015] The preparation method of the enhancer is as follows:

[0016] S01: irradiate the yttrium oxide in a proton irradiation box for 5-10 minutes at a power of 350W. After the irradiation is completed, preheat the yttrium oxide at 55-60°C for 10-15 minutes to obtain a preheated yttrium oxide body.

[0017] S02: Blend 2-4 parts of silane coupling agent KH550, 1-3 parts of chitosan solution with a mass fraction of 2-5%, and 4-7 parts of sodium dodecylbenzene sulfonate solution thoroughly;

[0018] Then, 3-5 parts of preheated yttrium oxide and 2-4 parts of B powder are added, and the blending and ball milling treatment is continued. The ball milling speed is 1500r / min, and the ball milling is performed for 2h. After the ball milling is completed, a yttrium oxide-based modifier is obtained;

[0019] S03: placing Si powder in a dopamine hydrochloride solution with an amount of 3-5 times the total amount of Si powder, and then adding carboxymethyl cellulose with an amount of 5-8% of the total amount of Si powder and blending them sufficiently to obtain a regulator;

[0020] S04: The regulator and the yttrium oxide-based modifier are stirred and modified in a weight ratio of 2:5. After the stirring is completed, the mixture is washed with water and dried to obtain a reinforcing agent.

[0021] Preferably, the mass fraction of the sodium dodecylbenzenesulfonate solution is 3-6%; the mass fraction of the dopamine hydrochloride solution is 4-7%.

[0022] Preferably, the particle size of the B powder is 10-15 um; the particle size of the Si powder is 2-5 um; the stirring speed of the stirring modification treatment is 450-550 r / min, and the stirring time is 30-40 min.

[0023] Preferably, the preparation method of the iron-based alloy is:

[0024] The alloy containing C, Cr, Fe, Mo, V and the reinforcing agent are sequentially added into the smelting furnace for smelting to form an iron-based alloy melt, which is then cast into a mold, cooled and formed, and then demolded to obtain an iron-based alloy ingot.

[0025] Preferably, the ceramic particles are also treated by ultrasonic immersion of a modifier;

[0026] The preparation method of the modifier is:

[0027] S11: immersing the silicon carbide whiskers into a lanthanum nitrate solution having a mass fraction of 4-6% and a value 3-5 times the total amount of the silicon carbide whiskers;

[0028] Then, 5-8% of the total amount of silicon carbide whiskers is added with silane coupling agent KH560, and the mixture is immersed and stirred sufficiently. The immersion speed is 550-750 r / min, and the immersion time is 30 min. After the immersion is completed, a lanthanum-doped whisker liquid is obtained;

[0029] S12: 2-5 parts of hydroxyapatite, 1-3 parts of flake graphene, 3-6 parts of sodium lignin sulfonate solution, 1-3 parts of citric acid and 0.50-0.75 parts of nano-silica sol are mixed and ball-milled at a speed of 1000-1500 r / min for 2 hours. After the ball-milling is completed, the mixture is washed with water and dried to obtain a modified additive;

[0030] S13: The lanthanum-doped whisker liquid and the modifying additive are mixed in a weight ratio of 7:3 to obtain a modifying agent.

[0031] Preferably, the mass fraction of the sodium lignin sulfonate solution is 2-5%;

[0032] Preferably, the immersion power of the ultrasonic immersion treatment is 350-400W, and the immersion time is 20-30min;

[0033] The invention also provides a composite reinforced wear-resistant material prepared by a method for preparing an iron-based ceramic composite reinforced wear-resistant material by a vacuum infiltration method.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] 1. The iron-based ceramic composite reinforced wear-resistant material of the present invention adopts ceramic particles, a binder, an activator, and paraffin particles to be mixed in a certain ratio, and then pressed and formed, and then sintered in a resistance furnace to form a ceramic prefabricated block with a porous structure. The high-temperature iron-based alloy liquid is vacuumed and infiltrated into the pores of the ceramic prefabricated body. The formed composite reinforced wear-resistant material has coordinated improvement in strength, toughness and wear resistance; the iron-based alloy adopts C, Cr, Fe, Mo, and V as the matrix raw materials, and the reinforcing agent is coordinated and matched, and the synergistic effect between the raw materials is adopted. At the same time, the ceramic particles are also ultrasonically immersed in the modifier for further coordination, so that the performance of the product is further improved;

[0036] 2. The reinforcing agent is yttrium oxide, which is first placed in a proton irradiation box for 5-10 minutes, and the irradiation power is 350W. After the irradiation, it is preheated at 55-60°C for 10-15 minutes. The activity of yttrium oxide is stimulated by irradiation and preheating. At the same time, silane coupling agent KH550, chitosan solution with a mass fraction of 2-5%, sodium dodecylbenzene sulfonate solution, and B powder are blended and adjusted. The interface between the raw materials of the system is enhanced by the coordination and matching between the raw materials, and then a regulator is combined to enhance the synergy. The Si powder in the regulator is first placed in a dopamine hydrochloride solution, and then mixed with carboxymethyl cellulose to obtain a regulator. The Si powder in the regulator is used to blend B powder and yttrium oxide, and then processed by the special process of the present invention, so that the organization grains can be refined and the grain structure can be strengthened in the alloy system, thereby obtaining an iron-based alloy combined with a ceramic body, and the strength, toughness and wear resistance of the product are further coordinated and improved, and the corrosion resistance and cold and hot shock resistance of the product are further improved;

[0037] 3. The modifier is made of silicon carbide whiskers, lanthanum nitrate solution with a mass fraction of 4-6%, and silane coupling agent KH560. The interface between the raw materials is enhanced through the coordination between the raw materials. At the same time, the whisker-like structure of the silicon carbide whiskers is distributed in the system, which enhances the wetting and interface improvement of the modifier on the ceramic particles. At the same time, the modifier additives are combined to enhance the improvement effect of the modifier on the ceramic particles, so that the product performance is further improved;

[0038] 4. The modified additive is made of hydroxyapatite, flaky graphene, sodium lignin sulfonate solution, citric acid and nano-silica sol, which are fully blended and ball-milled. The point-shaped hydroxyapatite is combined with the flaky graphene, which can better attach the modifier system to the surface of the ceramic particles, facilitate the lanthanum element in the modifier to penetrate and enhance the efficiency of the ceramic particle system, strengthen the organizational structure, and at the same time, the performance effect of the modifier on the ceramic particle system is further improved through the coordination of the raw materials of the modified additive with the whisker structure, thereby further enhancing the performance of the iron-based ceramic composite reinforced wear-resistant material. DETAILED DESCRIPTION

[0039] The following will clearly and completely describe the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of them. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0040] The preparation method of the iron-based ceramic composite reinforced wear-resistant material by the vacuum impregnation method in this embodiment includes the following steps:

[0041] Step 1: Mix ceramic particles with a particle size of 0.8 - 2.2 mm, a binder, an activator, and paraffin particles in proportion and stir to form a mixture.

[0042] Step 2: Place the mixture after stirring in Step 1 in a mold of a ceramic preform and press it into shape. Then put the mold into a resistance furnace, heat it to 120 °C, demold after 2 hours, and then sinter at a high temperature of 1250 °C for 12 hours to cause a phase change, and naturally cool to room temperature to obtain a ceramic preform with a multi-porous structure.

[0043] Step 3: Place the ceramic preform in a formed film shell, preheat it to 450 - 850 °C, and then place the preheated film shell in a vacuum furnace.

[0044] Step 4: Heat the iron-based alloy to 1520 - 1550 °C to melt it into a high-temperature iron-based alloy liquid, and pour it into the film shell of the vacuum furnace. Close the sealing cover of the vacuum furnace to keep it in a closed state. At the same time, start the vacuum pump to pump out the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic preform is pumped out, thereby enabling the iron-based alloy liquid to infiltrate into the pores of the ceramic preform. After keeping warm for 16 - 24 hours, cool it to room temperature to obtain the composite reinforced wear-resistant material of the present invention.

[0045] The iron-based alloy includes the following raw materials in parts by weight: 2 - 3.5 parts of C, 10 - 30 parts of Cr, 70 - 75 parts of Fe, 1.5 - 2 parts of Mo, and 1.5 - 2 parts of V.

[0046] The ratio of the ceramic particles, the binder, the activator, and the paraffin particles in this embodiment is (8 - 11):(2 - 3):(1 - 3):1; the activator is one or more of aluminum powder, silicon carbide powder, and tungsten carbide powder; the binder is an inorganic binder, and the inorganic binder is attapulgite clay.

[0047] The porosity of the ceramic preform with the multi-porous structure is 35 - 60%; the film shell preheated for forming is made of metal heat-resistant steel, non-metals, and composite materials.

[0048] The composite reinforced wear-resistant material of this embodiment also includes 8-13 parts of a reinforcing agent; the reinforcing agent is used for reinforcing and improving the iron-based alloy;

[0049] The preparation method of the enhancer is as follows:

[0050] S01: irradiate the yttrium oxide in a proton irradiation box for 5-10 minutes at a power of 350W. After the irradiation is completed, preheat the yttrium oxide at 55-60°C for 10-15 minutes to obtain a preheated yttrium oxide body.

[0051] S02: Blend 2-4 parts of silane coupling agent KH550, 1-3 parts of chitosan solution with a mass fraction of 2-5%, and 4-7 parts of sodium dodecylbenzene sulfonate solution thoroughly;

[0052] Then, 3-5 parts of preheated yttrium oxide and 2-4 parts of B powder are added, and the blending and ball milling treatment is continued. The ball milling speed is 1500r / min, and the ball milling is performed for 2h. After the ball milling is completed, a yttrium oxide-based modifier is obtained;

[0053] S03: placing Si powder in a dopamine hydrochloride solution with an amount of 3-5 times the total amount of Si powder, and then adding carboxymethyl cellulose with an amount of 5-8% of the total amount of Si powder and blending them thoroughly to obtain a regulator;

[0054] S04: The regulator and the yttrium oxide-based modifier are stirred and modified in a weight ratio of 2:5. After the stirring is completed, the mixture is washed with water and dried to obtain a reinforcing agent.

[0055] The mass fraction of the sodium dodecylbenzenesulfonate solution in this embodiment is 3-6%; the mass fraction of the dopamine hydrochloride solution is 4-7%.

[0056] The particle size of the B powder in this embodiment is 10-15um; the particle size of the Si powder is 2-5um; the stirring speed of the stirring modification treatment is 450-550r / min, and the stirring time is 30-40min.

[0057] The preparation method of the iron-based alloy of this embodiment is:

[0058] The alloy containing C, Cr, Fe, Mo, V and the reinforcing agent are sequentially added into the smelting furnace for smelting to form an iron-based alloy melt, which is then cast into a mold, cooled and formed, and then demolded to obtain an iron-based alloy ingot.

[0059] The ceramic particles of this embodiment are also treated by ultrasonic immersion of the modifier;

[0060] The preparation method of the modifier is:

[0061] S11: immersing the silicon carbide whiskers into a lanthanum nitrate solution having a mass fraction of 4-6% and a value 3-5 times the total amount of the silicon carbide whiskers;

[0062] Then, 5-8% of the total amount of silicon carbide whiskers is added with silane coupling agent KH560, and the mixture is immersed and stirred sufficiently. The immersion speed is 550-750 r / min, and the immersion time is 30 min. After the immersion is completed, a lanthanum-doped whisker liquid is obtained;

[0063] S12: 2-5 parts of hydroxyapatite, 1-3 parts of flake graphene, 3-6 parts of sodium lignin sulfonate solution, 1-3 parts of citric acid and 0.50-0.75 parts of nano-silica sol are mixed and ball-milled at a speed of 1000-1500 r / min for 2 hours. After the ball-milling is completed, the mixture is washed with water and dried to obtain a modified additive;

[0064] S13: The lanthanum-doped whisker liquid and the modifying additive are mixed in a weight ratio of 7:3 to obtain a modifying agent.

[0065] The mass fraction of the sodium lignin sulfonate solution in this embodiment is 2-5%;

[0066] The immersion power of the ultrasonic immersion treatment in this embodiment is 350-400W, and the immersion time is 20-30min;

[0067] The composite reinforced wear-resistant material prepared by the method for preparing an iron-based ceramic composite reinforced wear-resistant material by a vacuum infiltration method in this embodiment.

[0068] Example 1.

[0069] The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration in this embodiment comprises the following steps:

[0070] Step 1: Ceramic particles with a particle size of 0.8 mm are mixed with a binder, an activator, and paraffin particles in proportion and stirred to form a mixture;

[0071] Step 2: placing the mixture stirred in step 1 in a ceramic prefabricated block mold for pressing, then placing the mold in a resistance furnace, heating it to 120° C., demolding it after 2 hours, and then sintering it at a high temperature of 1250° C. for 12 hours to make it undergo a phase change, and naturally cooling it to room temperature to obtain a ceramic prefabricated block with a porous structure;

[0072] Step 3: Place the ceramic prefabricated block in the formed membrane shell, preheat it to 450°C, and then place the preheated membrane shell in a vacuum furnace;

[0073] Step 4: heating the iron-based alloy to 1520° C. to melt and form a high-temperature iron-based alloy liquid, and pouring the liquid into the membrane shell of the vacuum furnace, closing the sealing cover of the vacuum furnace to keep it in a closed state, and starting the vacuum pump to evacuate the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic prefabricated block is evacuated, thereby allowing the iron-based alloy liquid to infiltrate the pores of the ceramic prefabricated body, and then cooling to room temperature after keeping the temperature for 16 hours to obtain the composite reinforced wear-resistant material of the present invention;

[0074] The iron-based alloy includes the following raw materials in parts by weight: 2 parts of C, 10 parts of Cr, 70 parts of Fe, 1.5 parts of Mo, and 1.5 parts of V.

[0075] The ratio of ceramic particles to binder, activator, and paraffin particles in this embodiment is 8:2:1:1; the activator is aluminum powder; and the binder is an inorganic binder;

[0076] The porosity of the ceramic prefabricated block with a porous structure is 35%; the membrane shell preheated for molding is made of metal heat-resistant steel.

[0077] The composite reinforced wear-resistant material of this embodiment also includes 8 parts of reinforcing agent; the reinforcing agent is used for reinforcing and improving the iron-based alloy;

[0078] The preparation method of the enhancer is as follows:

[0079] S01: yttrium oxide is first placed in a proton irradiation box for 5 minutes, the irradiation power is 350W, and then preheated at 55°C for 10 minutes. After the preheating is completed, a preheated yttrium oxide body is obtained;

[0080] S02: 2 parts of silane coupling agent KH550, 1 part of 2% chitosan solution by mass and 4 parts of sodium dodecylbenzene sulfonate solution are mixed thoroughly;

[0081] Then, 3 parts of preheated yttrium oxide and 2 parts of B powder were added, and the blending and ball milling treatment was continued. The ball milling speed was 1500r / min, and the ball milling was performed for 2h. After the ball milling was completed, a yttrium oxide-based modifier was obtained.

[0082] S03: Si powder is first placed in a dopamine hydrochloride solution with an amount of 3 times the total amount of Si powder, and then carboxymethyl cellulose with an amount of 5% of the total amount of Si powder is added and mixed thoroughly to obtain a regulator;

[0083] S04: The regulator and the yttrium oxide-based modifier are stirred and modified in a weight ratio of 2:5. After the stirring is completed, the mixture is washed with water and dried to obtain a reinforcing agent.

[0084] The mass fraction of the sodium dodecylbenzenesulfonate solution in this embodiment is 3%; the mass fraction of the dopamine hydrochloride solution is 4%.

[0085] The particle size of the B powder in this embodiment is 10 μm; the particle size of the Si powder is 2 μm; the stirring speed of the stirring modification treatment is 450 r / min, and the stirring time is 30 min.

[0086] The preparation method of the iron-based alloy in this embodiment is as follows:

[0087] Add the C, Cr, Fe, Mo, V alloys and the reinforcing agent into the melting furnace in sequence for melting to make an iron-based alloy melt, then cast it into a mold, cool and form it, and then demold it to obtain an iron-based alloy ingot.

[0088] The ceramic particles in this embodiment are also treated by ultrasonic immersion with a modifier;

[0089] The preparation method of the modifier is as follows:

[0090] S11: Immerse the silicon carbide whiskers into a lanthanum nitrate solution with a mass fraction of 4% which is 3 times the total amount of the silicon carbide whiskers;

[0091] Subsequently, add 5% of the silane coupling agent KH560 based on the total amount of the silicon carbide whiskers, immerse and stir thoroughly, the immersion speed is 550 r / min, the immersion time is 30 min, and after the immersion is completed, a lanthanum-doped whisker liquid is obtained;

[0092] S12: Blend and ball-mill 2 parts of hydroxyapatite, 1 part of flaky graphene, 3 parts of sodium lignosulfonate solution, 1 part of citric acid and 0.50 part of nano-silica sol thoroughly, the ball-milling speed is 1000 r / min, ball-mill for 2 h, after the ball-milling is completed, wash with water and dry to obtain a modified additive;

[0093] S13: Mix and blend the lanthanum-doped whisker liquid and the modified additive according to a weight ratio of 7:3 thoroughly to obtain the modifier.

[0094] The mass fraction of the sodium lignosulfonate solution in this embodiment is 2%;

[0095] The immersion power of the ultrasonic immersion treatment in this embodiment is 350 W, and the immersion time is 20 min;

[0096] A composite reinforced wear-resistant material prepared by the preparation method of a vacuum impregnation method for manufacturing an iron-based ceramic composite reinforced wear-resistant material in this embodiment.

[0097] Example 2.

[0098] The preparation method of the vacuum impregnation method for manufacturing an iron-based ceramic composite reinforced wear-resistant material in this embodiment includes the following steps:

[0099] Step 1: Mix and stir ceramic particles with a particle size of 2.2 mm with a binder, an activator, and paraffin particles in proportion to make a mixture;

[0100] Step 2: placing the mixture stirred in step 1 in a ceramic prefabricated block mold for pressing, then placing the mold in a resistance furnace, heating it to 120° C., demolding it after 2 hours, and then sintering it at a high temperature of 1250° C. for 12 hours to make it undergo a phase change, and naturally cooling it to room temperature to obtain a ceramic prefabricated block with a porous structure;

[0101] Step 3: Place the ceramic prefabricated block in the formed membrane shell, preheat it to 850°C, and then place the preheated membrane shell in a vacuum furnace;

[0102] Step 4: heating the iron-based alloy to 1550° C. to melt and form a high-temperature iron-based alloy liquid, and pouring the high-temperature iron-based alloy liquid into the membrane shell of the vacuum furnace, closing the sealing cover of the vacuum furnace to keep it in a closed state, and starting the vacuum pump to evacuate the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic prefabricated block is evacuated, thereby allowing the iron-based alloy liquid to infiltrate the pores of the ceramic prefabricated body, and then cooling to room temperature after keeping warm for 24 hours to obtain the composite reinforced wear-resistant material of the present invention;

[0103] The iron-based alloy includes the following raw materials in parts by weight: 3.5 parts of C, 30 parts of Cr, 75 parts of Fe, 2 parts of Mo, and 2 parts of V.

[0104] The ratio of ceramic particles to binder, activator, and paraffin particles in this embodiment is 11:3:3:1; the activator is aluminum powder; and the binder is an inorganic binder;

[0105] The porosity of the ceramic prefabricated block with a porous structure is 60%; the membrane shell preheated for molding is made of metal heat-resistant steel.

[0106] The composite reinforced wear-resistant material of this embodiment also includes 3 parts of reinforcing agent; the reinforcing agent is used for reinforcing and improving the iron-based alloy;

[0107] The preparation method of the enhancer is as follows:

[0108] S01: irradiate the yttrium oxide in a proton irradiation box for 10 minutes at an irradiation power of 350W. After the irradiation is completed, preheat the yttrium oxide at 60°C for 15 minutes to obtain a preheated yttrium oxide body.

[0109] S02: Blend 4 parts of silane coupling agent KH550, 3 parts of 5% chitosan solution by mass, and 7 parts of sodium dodecylbenzene sulfonate solution thoroughly;

[0110] Then, 5 parts of preheated yttrium oxide and 4 parts of B powder were added, and the blending and ball milling treatment was continued. The ball milling speed was 1500r / min, and the ball milling was performed for 2h. After the ball milling was completed, a yttrium oxide-based modifier was obtained.

[0111] S03: First, place the Si powder in a hydrochloric acid dopamine solution that is 5 times the total amount of the Si powder. Subsequently, add carboxymethyl cellulose accounting for 8% of the total amount of the Si powder and mix well to obtain a regulator.

[0112] S04: Stir and modify the regulator and the yttrium-based modifier according to a weight ratio of 2:5. After stirring, wash with water and dry to obtain a reinforcing agent.

[0113] In this example, the mass fraction of the sodium dodecylbenzenesulfonate solution is 6%; the mass fraction of the hydrochloric acid dopamine solution is 7%.

[0114] In this example, the particle size of the B powder is 15 μm; the particle size of the Si powder is 5 μm; the stirring speed for the stirring and modification treatment is 550 r / min, and the stirring time is 40 min.

[0115] The preparation method of the iron-based alloy in this example is as follows:

[0116] Add the C, Cr, Fe, Mo, V alloy and the reinforcing agent into the melting furnace in sequence for melting to form an iron-based alloy melt. Then, cast it into a mold, cool and form, and then demold to obtain an iron-based alloy ingot.

[0117] In this example, the ceramic particles are also treated by ultrasonic immersion with the modifier.

[0118] The preparation method of the modifier is as follows:

[0119] S11: First, immerse the silicon carbide whiskers in a lanthanum nitrate solution with a mass fraction of 6% that is 5 times the total amount of the silicon carbide whiskers.

[0120] Subsequently, add silane coupling agent KH560 accounting for 8% of the total amount of the silicon carbide whiskers, immerse and stir well. The immersion speed is 750 r / min, and the immersion time is 30 min. After immersion, obtain a lanthanum-doped whisker solution.

[0121] S12: Mix 5 parts of hydroxyapatite, 3 parts of flaky graphene, 6 parts of lignosulfonate solution, 3 parts of citric acid and 0.75 part of nano-silica sol and ball-mill well. The ball-milling speed is 1500 r / min, and ball-mill for 2 h. After ball-milling, wash with water and dry to obtain a modified additive.

[0122] S13: Mix the lanthanum-doped whisker solution and the modified additive according to a weight ratio of 7:3 and mix well to obtain a modifier.

[0123] In this example, the mass fraction of the lignosulfonate solution is 5%.

[0124] In this example, the immersion power for the ultrasonic immersion treatment is 400 W, and the immersion time is 30 min.

[0125] The composite reinforced wear-resistant material prepared by the preparation method of a vacuum infiltration method for manufacturing an iron-based ceramic composite reinforced wear-resistant material in this embodiment.

[0126] Example 3.

[0127] The preparation method of the vacuum infiltration method for manufacturing an iron-based ceramic composite reinforced wear-resistant material in this embodiment includes the following steps:

[0128] Step 1: Mix ceramic particles with a particle size of 1.5 mm with a binder, an activator, and paraffin particles in proportion and stir to form a mixture;

[0129] Step 2: Place the stirred mixture in Step 1 in a mold of a ceramic preform, press it into shape, then put the mold into a resistance furnace, heat it to 120 °C, demold after 2 hours, and then sinter it at a high temperature of 1250 °C for 12 hours to cause a phase change, and naturally cool it to room temperature to obtain a ceramic preform with a porous structure;

[0130] Step 3: Place the ceramic preform in a formed film shell, preheat it to 450 - 850 °C, and then place the preheated film shell in a vacuum furnace;

[0131] Step 4: Heat the iron-based alloy to 1535 °C to melt it into a high-temperature iron-based alloy liquid, pour it into the film shell of the vacuum furnace, close the sealing cover of the vacuum furnace to keep it in a closed state, and at the same time start the vacuum pump to pump out the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic preform is pumped out, so that the iron-based alloy liquid infiltrates into the pores of the ceramic preform, and after keeping warm for 20 hours, it is cooled to room temperature to obtain the composite reinforced wear-resistant material of the present invention;

[0132] Among them, the iron-based alloy includes the following raw materials in parts by weight: 3.0 parts of C, 20 parts of Cr, 72.5 parts of Fe, 1.8 parts of Mo, and 1.7 parts of V.

[0133] The ratio of the ceramic particles to the binder, the activator, and the paraffin particles in this embodiment is 10:2.5:2:1; the activator is silicon carbide powder; the binder is an inorganic binder;

[0134] The porosity of the ceramic preform with the porous structure is 38.5%; the film shell used for preheating and forming is a metal heat-resistant steel.

[0135] The composite reinforced wear-resistant material in this embodiment further includes 11 parts of a reinforcing agent; the reinforcing agent is used for the reinforcing and improving treatment of the iron-based alloy;

[0136] Among them, the preparation method of the reinforcing agent is:

[0137] S01: First, place yttrium oxide in a proton irradiation chamber and irradiate it for 7.5 min at an irradiation power of 350 W. After the irradiation ends, preheat it at 58 °C for 12.5 min. After the preheating ends, obtain the preheated yttrium oxide body;

[0138] S02: Blend 3 parts of silane coupling agent KH550, 2 parts of a 3.5% chitosan solution by mass fraction, and 5.5 parts of a sodium dodecylbenzenesulfonate solution thoroughly;

[0139] Subsequently, add 4 parts of the preheated yttrium oxide body and 3 parts of B powder, and continue to blend and ball-mill. The ball-milling speed is 1500 r / min, and ball-mill for 2 h. After the ball-milling ends, obtain the modifier based on yttrium oxide;

[0140] S03: First, place Si powder in a hydrochloric acid dopamine solution that is 4 times the total amount of Si powder. Subsequently, add 6.5% of the total amount of Si powder of carboxymethyl cellulose and blend thoroughly to obtain a regulator;

[0141] S04: Stir and modify the regulator and the modifier based on yttrium oxide according to a weight ratio of 2:5. After the stirring ends, wash with water and dry to obtain a reinforcing agent.

[0142] In this embodiment, the mass fraction of the sodium dodecylbenzenesulfonate solution is 4.5%; the mass fraction of the hydrochloric acid dopamine solution is 5.5%.

[0143] In this embodiment, the particle size of the B powder is 12.5 μm; the particle size of the Si powder is 3.5 μm; the stirring speed of the stirring and modification treatment is 500 r / min, and the stirring time is 35 min.

[0144] The preparation method of the iron-based alloy in this embodiment is as follows:

[0145] Add the C, Cr, Fe, Mo, V alloy and the reinforcing agent to the melting furnace in sequence for melting to form an iron-based alloy melt. Then, pour it into a mold, cool and form, and then demold to obtain an iron-based alloy ingot.

[0146] In this embodiment, the ceramic particles are also treated by ultrasonic immersion with the modifier;

[0147] The preparation method of the modifier is as follows:

[0148] S11: First, immerse silicon carbide whiskers in a 5% lanthanum nitrate solution that is 4 times the total amount of silicon carbide whiskers;

[0149] Subsequently, add 6.5% of the total amount of silicon carbide whiskers of silane coupling agent KH560, immerse and stir thoroughly. The immersion speed is 600 r / min, and the immersion time is 30 min. After the immersion ends, obtain the lanthanum-doped whisker liquid;

[0150] S12: Blend 3.5 parts of hydroxyapatite, 2 parts of flaky graphene, 4.5 parts of sodium lignosulfonate solution, 2 parts of citric acid, and 0.60 part of nano-silica sol thoroughly by ball milling. The ball milling speed is 1,250 r / min, and ball mill for 2 h. After ball milling, wash with water and dry to obtain a modified additive.

[0151] S13: Mix the lanthanum-doped whisker liquid and the modified additive thoroughly according to a weight ratio of 7:3 to obtain a modifier.

[0152] In this example, the mass fraction of the sodium lignosulfonate solution is 3.5%.

[0153] In this example, the immersion power of the ultrasonic immersion treatment is 370 W, and the immersion time is 25 min.

[0154] A composite reinforced wear-resistant material prepared by the preparation method of a vacuum infiltration method for manufacturing an iron-based ceramic composite reinforced wear-resistant material in this example.

[0155] Comparative Example 1.

[0156] The difference from Example 3 is that no reinforcing agent is added to the iron-based alloy.

[0157] Comparative Example 2.

[0158] The difference from Example 3 is that no regulator treatment is added during the preparation of the reinforcing agent.

[0159] Comparative Example 3.

[0160] The difference from Example 3 is that the regulator is replaced with Si powder.

[0161] Comparative Example 4.

[0162] The difference from Example 3 is that no yttrium-based modifier is added to the reinforcing agent.

[0163] Comparative Example 5.

[0164] The difference from Example 3 is that no preheated yttrium oxide body is added during the preparation of the yttrium-based modifier.

[0165] Comparative Example 6.

[0166] The difference from Example 3 is that no B powder and silane coupling agent KH550 are added during the preparation of the yttrium-based modifier.

[0167] Comparative Example 7.

[0168] The difference from Example 3 is that no modifier treatment is used for the ceramic particles.

[0169] Comparative Example 8.

[0170] The difference from Example 3 is that no modified additive is added to the modifier.

[0171] Comparative Example 9.

[0172] The difference from Example 3 is that no silicon carbide whiskers are added to the lanthanum-doped whisker liquid.

[0173] Comparative Example 10.

[0174] The difference from Example 3 is that the preparation method of the modifier is different:

[0175] 3.5 parts of hydroxyapatite, 2 parts of flaky graphene, 4.5 parts of sodium lignin sulfonate solution, 2 parts of citric acid and 0.65 parts of nano-silica sol were fully ball-milled at a ball-milling speed of 1250 r / min for 2 hours to obtain a modifier.

[0176] The strength, toughness and wear resistance of the products of Examples 1 to 3 and Comparative Examples 1 to 10 were tested, and the test results are as follows:

[0177]

[0178]

[0179] It can be seen from Comparative Examples 1 to 10 and Examples 1 to 3 that;

[0180] The product of Example 3 has excellent fracture toughness, as well as excellent bending strength and wear resistance, and the three can be improved in a coordinated manner. The product performance of Example 3 is superior to the product performance of Comparative Examples 1-10.

[0181] The product was placed in 2% hydrochloric acid mist for 1 hour, then placed at 120°C with an impact strength of 10Mp for 5 minutes, and then at -5°C with an impact strength of 10Mp for 5 minutes. The above test is one cycle, and a total of 10 cycles were performed to test the corrosion resistance and thermal shock resistance of the product. The test results are as follows

[0182]

[0183]

[0184] It can be seen from Comparative Examples 1 to 10 and Example 3 that

[0185] Without adding reinforcing agent to iron-based alloy and without using modifier to treat ceramic particles, the performance of the product has a significant trend of deterioration. The synergistic effect of the two is the most significant.

[0186] In the preparation of the reinforcing agent, no regulator was added for treatment, the regulator was replaced by Si powder, no yttrium oxide-based modifier was added to the reinforcing agent, no preheated yttrium oxide body was added in the preparation of the yttrium oxide-based modifier, and no B powder and silane coupling agent KH550 were added in the preparation of the yttrium oxide-based modifier. The performance of the products showed a trend of deterioration to varying degrees. The product performance effect was most significant when the regulator obtained by the method of the present invention was used in combination with the yttrium oxide-based modifier obtained by the method of the present invention. The effects of other methods were not as obvious as those of the present invention.

[0187] When no modifying additive is added to the modifier, no silicon carbide whisker is added to the lanthanum-doped whisker liquid, and the preparation methods of the modifier are different, the performance of the product tends to deteriorate. When no modifying additive is added, the performance of the product tends to deteriorate significantly. The modifier obtained by the method of the present invention has the most significant product performance effect.

[0188] Since the modified additives have a significant impact on the performance of the product, further research is needed:

[0189] 3.5 parts of hydroxyapatite, 2 parts of flake graphene, 4.5 parts of sodium lignin sulfonate solution, 2 parts of citric acid and 0.65 parts of nano-silica sol were fully blended and ball-milled at a ball-milling speed of 1250 r / min for 2 hours. After the ball-milling was completed, the mixture was washed with water and dried to obtain a modified additive.

[0190] Experimental example 1.

[0191] The only difference from Example 3 is that hydroxyapatite is not added to the modification additive.

[0192] Experimental example 2.

[0193] The only difference from Example 3 is that no flake graphene is added to the modifying additive.

[0194] Experimental Example 3.

[0195] The only difference from Example 3 is that the sodium lignin sulfonate solution is replaced by deionized water.

[0196] Experimental Example 4.

[0197] The only difference from Example 3 is that citric acid and nano-silica sol are not added to the modified additive.

[0198] Based on the corrosion resistance and thermal shock resistance tests, the performance of product experimental examples 1-4 was further tested as follows:

[0199]

[0200] It can be seen from Experimental Examples 1-4 that when flaky graphene is not added to the modified additive, the performance of the product is most affected by the modified additive. Next is the case where hydroxyapatite is not added. At the same time, when deionized water is used instead of sodium lignosulfonate solution in the product, and citric acid and nano-silica sol are not added to the modified additive, the performance of the product shows a deteriorating trend. The modified additive obtained by the mutual cooperation of citric acid, sodium lignosulfonate solution, and nano-silica sol with hydroxyapatite and flaky graphene, through the mutual coordination and synergy of the raw materials, and common synergy, has the most significant effect on the product performance. None of the raw materials in the modified additive can be missing. Using other methods to replace them is not as effective as the present invention.

[0201] For those skilled in the art, it is obvious that the present invention is not limited to the details of the above exemplary embodiments, and without departing from the spirit or basic characteristics of the present invention, the present invention can be implemented in other specific forms. Therefore, from any point of view, the embodiments should be regarded as exemplary and non-limiting. The scope of the present invention is defined by the appended claims rather than the above description. Therefore, all changes falling within the meaning and scope of the equivalent elements of the claims are intended to be encompassed within the present invention.

[0202] In addition, it should be understood that although this specification is described according to embodiments, not every embodiment only contains an independent technical solution. This narrative way of the specification is only for clarity. Those skilled in the art should regard the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration, characterized in that: The following steps are involved: Step 1: Ceramic particles with a particle size of 0.8-2.2 mm, a binder, an activator, and paraffin particles are mixed and stirred in proportion to form a mixture; Step 2: placing the mixture stirred in step 1 in a ceramic prefabricated block mold for pressing, then placing the mold in a resistance furnace, heating it to 120° C., demolding it after 2 hours, and then sintering it at a high temperature of 1250° C. for 12 hours to make it undergo a phase change, and naturally cooling it to room temperature to obtain a ceramic prefabricated block with a porous structure; Step 3: Place the ceramic prefabricated block in the formed membrane shell, preheat it to 450-850°C, and then place the preheated membrane shell in a vacuum furnace; Step 4: heating the iron-based alloy to 1520-1550°C to melt and form a high-temperature iron-based alloy liquid, and pouring it into the membrane shell of the vacuum furnace, closing the sealing cover of the vacuum furnace to keep it in a closed state, and starting the vacuum pump to evacuate the air in the vacuum furnace to a vacuum state, so that the air in the pores of the ceramic prefabricated block is evacuated, so that the iron-based alloy liquid infiltrates into the pores of the ceramic prefabricated body, keeping the temperature for 16-24 hours, and then cooling to room temperature to obtain a composite reinforced wear-resistant material; The iron-based alloy comprises the following raw materials in parts by weight: 2-3.5 parts of C, 10-30 parts of Cr, 70-75 parts of Fe, 1.5-2 parts of Mo, and 1.5-2 parts of V; The composite reinforced wear-resistant material also includes 8-13 parts of a reinforcing agent; the reinforcing agent is used for reinforcing and improving the iron-based alloy; The preparation method of the enhancer is as follows: S01: irradiate the yttrium oxide in a proton irradiation box for 5-10 minutes at a power of 350W. After the irradiation is completed, preheat the yttrium oxide at 55-60°C for 10-15 minutes to obtain a preheated yttrium oxide body. S02: Blend 2-4 parts of silane coupling agent KH550, 1-3 parts of chitosan solution with a mass fraction of 2-5%, and 4-7 parts of sodium dodecylbenzene sulfonate solution thoroughly; Then, 3-5 parts of preheated yttrium oxide and 2-4 parts of B powder are added, and the blending and ball milling treatment is continued. The ball milling speed is 1500r / min, and the ball milling is performed for 2h. After the ball milling is completed, a yttrium oxide-based modifier is obtained; S03: placing Si powder in a dopamine hydrochloride solution with an amount of 3-5 times the total amount of Si powder, and then adding carboxymethyl cellulose with an amount of 5-8% of the total amount of Si powder and blending them sufficiently to obtain a regulator; S04: stirring and modifying the regulator and the yttrium oxide-based modifier in a weight ratio of 2:5, washing with water and drying after the stirring is completed to obtain a reinforcing agent; The preparation method of the iron-based alloy is: The alloy containing C, Cr, Fe, Mo, V and the reinforcing agent are sequentially added into a smelting furnace for smelting to form an iron-based alloy melt, which is then cast into a mold, cooled and formed, and then demolded to obtain an iron-based alloy ingot; The ceramic particles are also treated by ultrasonic immersion of a modifier; The preparation method of the modifier is: S11: immersing the silicon carbide whiskers into a lanthanum nitrate solution having a mass fraction of 4-6% and a value 3-5 times the total amount of the silicon carbide whiskers; Then, 5-8% of the total amount of silicon carbide whiskers is added with silane coupling agent KH560, and the mixture is immersed and stirred sufficiently. The immersion speed is 550-750 r / min, and the immersion time is 30 min. After the immersion is completed, a lanthanum-doped whisker liquid is obtained; S12: 2-5 parts of hydroxyapatite, 1-3 parts of flake graphene, 3-6 parts of sodium lignin sulfonate solution, 1-3 parts of citric acid and 0.50-0.75 parts of nano-silica sol are mixed and ball-milled at a speed of 1000-1500 r / min for 2 hours. After the ball-milling is completed, the mixture is washed with water and dried to obtain a modified additive; S13: The lanthanum-doped whisker liquid and the modifying additive are mixed in a weight ratio of 7:3 to obtain a modifying agent.

2. The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration according to claim 1, characterized in that: The ratio of the ceramic particles to the binder, activator and paraffin particles is (8-11):(2-3):(1-3):1; wherein the activator is one of aluminum powder, silicon carbide powder and tungsten carbide powder; and the binder is an inorganic binder; The porosity of the ceramic prefabricated block with a porous structure is 35-60%; the membrane shell preheated for molding is made of metal heat-resistant steel.

3. The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration according to claim 1, characterized in that: The mass fraction of the sodium dodecylbenzenesulfonate solution is 3-6%; the mass fraction of the dopamine hydrochloride solution is 4-7%.

4. The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration according to claim 1, characterized in that: The particle size of the B powder is 10-15 μm; the particle size of the Si powder is 2-5 μm; the stirring speed of the stirring modification treatment is 450-550 r / min, and the stirring time is 30-40 min.

5. The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration according to claim 1, characterized in that: The mass fraction of the sodium lignin sulfonate solution is 2-5%.

6. The method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration according to claim 1, characterized in that: The immersion power of the ultrasonic immersion treatment is 350-400W, and the immersion time is 20-30min.

7. A composite reinforced wear-resistant material prepared by the method for preparing an iron-based ceramic composite reinforced wear-resistant material by vacuum infiltration method as claimed in any one of claims 1 to 6.

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