CN111455253A - Titanium carbide-based metal ceramic thermal spraying powder and preparation method thereof - Google Patents
Titanium carbide-based metal ceramic thermal spraying powder and preparation method thereof Download PDFInfo
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1003—Use of special medium during sintering, e.g. sintering aid
- B22F3/1007—Atmosphere
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- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- C23C24/00—Coating starting from inorganic powder
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- B22F9/00—Making metallic powder or suspensions thereof
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- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
Abstract
The invention provides titanium carbide-based metal ceramic thermal spraying powder and a preparation method thereof, and solves the technical problems that the titanium carbide-based metal ceramic powder prepared in the prior art has poor component uniformity, low powder density, non-uniform metal coating and poor sphericity. The preparation method comprises the following main materials in percentage by weight: TiC 20-40%; 20% -30% of TiN; WC10%‑20%；Mo22% -6% of C; co10% -30%; 10% -30% of Ni; the sum of the weight percentages of the main materials is 100 percent. The titanium carbide-based metal ceramic thermal spraying powder prepared by the method has good component uniformity, high powder density, uniform metal coating, high sphericity and good fluidity; and the application of the slow sintering method can realize the mass continuous production.
Description
Technical Field
The invention relates to thermal spraying powder, in particular to titanium carbide-based metal ceramic thermal spraying powder.
Background
For thermal spraying powder, the manufacturing process is wide in variety, and the selection of the manufacturing process directly affects the performance of the thermal spraying powder, and the methods generally adopted for preparing ceramic powder at present include melting crushing, sintering crushing, spray drying, self-propagating high-temperature synthesis sol-gel method gas phase method and the like.
The spray drying method is the most commonly used powder preparation method at present, which can bond small particles of any material by using a binder to form large spherical agglomerated particles, and has large compatibility with the powder type, but the spray drying method is not a cheap method for preparing the powder, and meanwhile, the process requires long time for searching and optimizing the densification preparation of the metal ceramic composite powder with large difference of melting points.
Cermet powders produced by sintering or melting have irregular shapes which deteriorate their flowability, and in order to improve the flowability of the powders, the powders are subjected to a post-treatment such as spheroidization in a flame or a plasma arc, but pores are formed in the interior of the powders after the spheroidization.
The self-propagating high-temperature synthesis is a combustion reaction, the exothermic reaction in the reaction can maintain the chemical reaction of the self-propagating high-temperature synthesis, and the reaction powder is gradually converted into the required material, but the reactant is generally required to be prepared into a rod shape, and the homogenization of the prepared powder is difficult to realize in the process of preparing the metal ceramic composite powder.
Furthermore, the powder preparation methods described above all require a high temperature process, which greatly increases the probability of new phases being produced and the risk of introducing impurities.
In industrial production conditions requiring surface corrosion resistance and wear resistance, a metal ceramic coating is often adopted to strengthen the surface so as to meet the application requirements; the metal ceramic is carbide-base metal ceramic, which is TiC, WC, Cr3C2The carbide is used as ceramic phase and is prepared by mixing a certain amount of metal or alloy powder. Gold for sprayingThe ceramic powder needs to have good fluidity and sphericity, higher apparent density and certain mechanical strength. For different use conditions, the morphology of the powder, the component distribution of the powder particles and the like need to be regulated and controlled.
Chinese patents CN102363876B, CN10876908B, CN10884892A, and CN 108326319 a describe a method for preparing granulated WC-Co powder for thermal spraying, which is a target product WC-Co powder having better sphericity, uniform metal coating, and uniform powder particle size, prepared by continuous improvement on the basic processes of wet grinding, granulation, and sintering. Although the WC-Co coating has high hardness and can resist particle abrasion or contact abrasion in the using process, the low corrosion resistance and oxidation resistance of the WC-Co coating greatly limit the using range of the WC-Co coating. Chinese patent CN 101451225A introduces a nickel-based Cr-containing alloy3C2The spray powder for corrosion-resistant coatings and the process for its preparation by Cr3C2The addition of (2) can greatly improve the acid corrosion resistance and the oxidation resistance of the coating surface. The Cr-containing compounds3C2The hardness and wear resistance of the coating are generally low, and the coating cannot be used for a long time under the application condition that the coating needs to bear abrasion and large load.
The TiC-based cermet material has quite excellent hardness and wear resistance and good chemical stability, is generally used in environments with severe use conditions such as cutting tools, dies and drilling wells, but has not been applied as a coating so far because TiC has poor wettability with most metals, so that an interface between a coating and a substrate with good bonding and compactness cannot be obtained, and in addition, the thermal spraying preparation process of the coating is difficult due to the high melting point of TiC. The performance and the appearance of the powder for coating directly influence the performance of the coating after spraying.
The applicant has found that the prior art has at least the following technical problems:
the titanium carbide-based metal ceramic powder prepared in the prior art has the problems of poor component uniformity, low powder density, non-uniform metal coating and poor sphericity.
Disclosure of Invention
The invention aims to provide titanium carbide-based metal ceramic thermal spraying powder and a preparation method thereof, and aims to solve the technical problems that the titanium carbide-based metal ceramic powder prepared in the prior art is poor in component uniformity, low in powder density, non-uniform in metal coating and poor in sphericity. The technical effects that can be produced by the preferred technical scheme in the technical schemes provided by the invention are described in detail in the following.
In order to achieve the purpose, the invention provides the following technical scheme:
the invention provides titanium carbide-based cermet thermal spraying powder, which is prepared from the following main materials in percentage by weight:
the sum of the weight percentages of the main materials is 100 percent.
Further, the weight percentages of the main materials are respectively as follows:
the sum of the weight percentages of the main materials is 100 percent.
Further, the weight percentages of the main materials are respectively as follows:
furthermore, the preparation method also comprises auxiliary materials, wherein the auxiliary materials comprise a binder and a wet grinding medium, and the addition amount of the binder is 3-6% of the total weight of the main materials.
The invention provides a preparation method of titanium carbide-based cermet thermal spraying powder, which comprises the following steps:
(1) wet grinding:
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and carrying out wet milling to obtain uniformly mixed slurry;
② drying the slurry obtained in step ① to obtain a dry and uniform mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 30-50 deg.C, starting low speed stirring, simultaneously adding alcohol in form of uniform spraying, stopping adding alcohol and stirring after 10min, taking out the powder and pouring into a 80 mesh screen, applying pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100 mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100 mesh screen is the granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen mesh to continuously obtain the granulated TiC-based metal ceramic powder for later use;
③ placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace to remove a binder, so as to obtain granulated TiC-based metal ceramic powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method or a fast sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder.
Further, in the step (3), the vacuum degreasing comprises the following steps:
①, placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to be below 0.01Pa, heating the powder from room temperature to 200-300 ℃ at the heating rate of 4-6 ℃/min, and then keeping the temperature for 1.5-2.5 h;
② continuously heating to 550-650 deg.C at a heating rate of 4-6 deg.C/min, and keeping the temperature for 4.5-5.5 h;
③ and finally cooling to room temperature along with the furnace to obtain the granular TiC-based metal ceramic powder.
Further, in the step (4), the slow sintering method includes the following steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 500-600 ℃ at the heating rate of 8-12 ℃/min, and then preserving heat for 1-2 h;
② is heated to 700-800 ℃ at the heating rate of 4-6 ℃/min, and then the temperature is kept for 1-2 h;
③ heating to 1100-1200 deg.C at a heating rate of 4-6 deg.C/min, and holding for 2-4 h;
④ cooling with furnace to obtain pre-sintered alloyed titanium carbide-based cermet thermal spraying powder;
the rapid sintering method comprises the following steps: placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying current to the granulated TiC-based metal ceramic powder, simultaneously heating the temperature in the furnace at the heating rate of 8-12 ℃/min, and stopping applying the current and heating when the temperature is raised to 850-950 ℃; finally, the titanium carbide-based cermet thermal spraying powder which is presintered and alloyed is obtained by furnace cooling.
Further, in the step (1), the added adhesive is paraffin or polyethylene glycol, and the adding amount of the adhesive is 3% -6% of the total weight of the main materials.
Further, in the step (1), during wet grinding, the material of the grinding ball is hard alloy, and the wet grinding rotating speed is 60r/min-100 r/min.
Further, in the step (2), the applied pressure is 2N-8N when the mixture is sieved by an 80-mesh sieve.
Based on the technical scheme, the embodiment of the invention can at least produce the following technical effects:
the titanium carbide-based cermet thermal spraying powder and the preparation method provided by the invention can realize simple, convenient and efficient preparation of powder for TiC-based cermet spraying, and the regulation and control of the shape, granularity, component distribution and the like of the powder are simple and easy to realize by the preparation method; and the application of the slow sintering method can realize the continuous production in large batch; WC-Co coating and Cr3C2And (4) coating.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a micrograph of T1 powder prepared according to example 1 of the present invention;
FIG. 2 is a micrograph of T3 powder prepared according to example 3 of the present invention;
fig. 3 is a side view of the coating of T1 powder prepared according to example 1 of the present invention sprayed onto the surface of a steel substrate by a laser cladding process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
First, preparation example:
1. main materials:
titanium carbide-based cermet thermal spray powders were prepared in examples 1 to 9, with the amounts (in weight%) of the major ingredients shown in table 1 below;
TiC, TiN, WC and Mo in main materials2C. Co and Ni are powder, the grain diameter of TiC is 2-4 μm, the grain diameter of TiN is 2-4.5 μm, the grain diameter of WC is 1-2.5 μm, Mo2The grain size of C is 2-4 μm, the grain size of Co is 1-4 μm, the grain size of Ni is 1-4 μm, the grain size of the main material in examples 1-9 is shown in the following table 2:
table 1 examples main ingredient table
TABLE 2 particle size of the major material
2. The preparation method comprises the following steps:
example 1:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 48 hours at a rotating speed of 60r/min to obtain uniformly mixed slurry;
wherein the adhesive is paraffin wax, and the addition amount of the adhesive is TiC, TiN, WC and Mo2C. 4% of the total weight of Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
②, drying the slurry obtained in step ① in a vacuum oven with the vacuum degree of 70Pa and the drying temperature of 80 ℃ for 4 hours to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 30r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 6N pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying at 50 ℃, wherein the vacuum degree is 80Pa and the drying time is 5h to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
①, loosely packing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing the corundum boat in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to 0.01Pa, heating the corundum boat from room temperature to 250 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 2 hours;
② continuously heating to 550 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder; the method comprises the following specific steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 600 ℃ at the heating rate of 10 ℃/min, and then preserving heat for 1.5 h;
② heating to 800 deg.C at a rate of 5 deg.C/min, and maintaining for 1.5 h;
③ heating to 1150 deg.C at a heating rate of 5 deg.C/min, and holding for 3 hr;
④ and finally cooling the furnace to obtain the presintered alloyed titanium carbide-based cermet thermal spraying powder with the number T1.
As shown in FIG. 1, the morphology of the titanium carbide-based cermet thermal spray powder prepared in example 1 was found to have good sphericity and smooth and uniform surface.
Fig. 3 shows the profile of the side surface of the coating layer of the titanium carbide-based cermet thermal spray powder prepared in example 1 sprayed on the surface of the steel substrate by the laser cladding process, and it can be seen from the profile of the coating layer that the coating layer sprayed with the powder prepared by the method of the present invention is fully densified, has no pores, has uniform size and uniform distribution of hard phases, has good wettability to the hard particles, and does not show any hard phase agglomeration.
Example 2:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 4.5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 48 hours at a rotating speed of 60r/min to obtain uniformly mixed slurry;
wherein the adhesive is paraffin or polyethylene glycol, and the addition amount of the adhesive is TiC, TiN, WC and Mo2C. 4% of the total weight of Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
②, drying the slurry obtained in step ① in a vacuum oven with the vacuum degree of 70Pa and the drying temperature of 80 ℃ for 4 hours to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 30r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 8N pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying at 50 ℃, wherein the vacuum degree is 100Pa and the drying time is 5h, so as to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
①, loosely packing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing the corundum boat in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to be below 0.01Pa, heating the TiC-based cermet powder from room temperature to 250 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 2 hours;
② continuously heating to 550 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder; the method comprises the following specific steps:
① placing the TiC base cermet powder in step (3) into a vacuum furnace, vacuumizing, and charging N2When the atmosphere reaches 100KPa, firstly heating to 600 ℃ at the heating rate of 10 ℃/min, and then preserving the heat for 2 h;
② heating to 800 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 2 h;
③ heating to 1150 deg.C at a heating rate of 5 deg.C/min, and holding for 4 hr;
④ and finally cooling the furnace to obtain the presintered alloyed titanium carbide-based cermet thermal spraying powder with the number T2.
Example 3:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 4.5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 48 hours at a rotating speed of 60r/min to obtain uniformly mixed slurry;
wherein the adhesive is paraffin or polyethylene glycol, and the addition amount of the adhesive is TiC, TiN, WC and Mo2C. 4% of the total weight of Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
②, drying the slurry obtained in step ① in a vacuum oven with the vacuum degree of 70Pa and the drying temperature of 80 ℃ for 4 hours to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 30r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 2N pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying at 50 ℃, wherein the vacuum degree is 50Pa and the drying time is 5h, so as to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
① loose placing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing in a vacuum degreasing furnace, heating from room temperature to 250 ℃ at a heating rate of 5 ℃/min after the vacuum degree in the furnace is pumped to 0.01Pa, and then keeping the temperature for 2 hours;
② continuously heating to 550 ℃ at the heating rate of 5 ℃/min, and then keeping the temperature for 5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a rapid sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method specifically comprises the following steps:
placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a corundum boat, placing the corundum boat into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying a direct-current electric field strength of 30V/cm to the granulated TiC-based metal ceramic powder, simultaneously heating the granulated TiC-based metal ceramic powder at a heating rate of 10 ℃/min, and when the temperature is raised to 850 ℃, carrying out a strong reaction on particles so as to carry out instant densification, and stopping applying current and heating; finally, the pre-sintered alloyed titanium carbide-based cermet thermal spraying powder is obtained along with furnace cooling, and the number of the powder is T3.
As shown in FIG. 2, the morphology of the titanium carbide-based cermet thermal spray powder prepared in example 3 was shown to have good sphericity and smooth and uniform surface.
Example 4:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 40 hours at a rotating speed of 80r/min to obtain uniformly mixed slurry;
wherein, the adhesive is paraffin or polyethylene glycol, and the addition of the adhesive is 6 percent of the total weight of TiC, TiN, WC, Mo2C, Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
②, drying the slurry obtained in step ① in a vacuum oven with the vacuum degree of 70Pa and the drying temperature of 80 ℃ for 3.5 to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 30-50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 40r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 5N pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying at 50 ℃, wherein the vacuum degree is 60Pa and the drying time is 6h to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
① loose placing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing in a vacuum degreasing furnace, heating from room temperature to 300 ℃ at a heating rate of 4 ℃/min after the vacuum degree in the furnace is pumped to 0.01Pa, and then keeping the temperature for 2.5 h;
② continuously heating to 550 ℃ at the heating rate of 6 ℃/min, and then keeping the temperature for 4.5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method to obtain presintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method comprises the following specific steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 600 ℃ at the heating rate of 12 ℃/min, and then preserving heat for 1 h;
② heating to 800 ℃ at the heating rate of 6 ℃/min, and then keeping the temperature for 2 h;
③ heating to the final sintering temperature of 1200 ℃ at the heating rate of 6 ℃/min, and then keeping the temperature for 2 h;
④ and cooling in furnace to obtain the pre-sintered alloyed titanium carbide-based cermet thermal spraying powder.
Example 5:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 5.5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 60 hours at a rotating speed of 100r/min to obtain uniformly mixed slurry;
wherein, the adhesive is paraffin or polyethylene glycol, and the addition of the adhesive is 3 percent of the total weight of TiC, TiN, WC, Mo2C, Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
②, drying the slurry obtained in step ① in a vacuum oven with the vacuum degree of 70Pa and the drying temperature of 80 ℃ for 4.5h to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 30-50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 45r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 3N pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying at 50 ℃, wherein the vacuum degree is 70Pa and the drying time is 7h to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
① loose placing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to below 0.01Pa, heating from room temperature to 200 ℃ at the heating rate of 6 ℃/min, and then keeping the temperature for 1.5 h;
② continuously heating to 650 deg.C at a heating rate of 4 deg.C/min, and keeping the temperature for 5.5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method to obtain presintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method comprises the following specific steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 500 ℃ at the heating rate of 8 ℃/min, and then preserving heat for 2 hours;
② heating to 700 deg.C at a heating rate of 4 deg.C/min, and maintaining for 2 h;
③ heating to 1100 deg.C at a heating rate of 4 deg.C/min, and holding for 4 hr;
④ and cooling in furnace to obtain the pre-sintered alloyed titanium carbide-based cermet thermal spraying powder.
Example 6:
the method comprises the following steps:
(1) wet milling (ball to feed ratio: 4.5: 1):
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and performing ball milling for 55 hours at a rotating speed of 70r/min to obtain uniformly mixed slurry;
wherein, the adhesive is paraffin or polyethylene glycol, and the addition amount of the adhesive is 3 to 6 percent of the total weight of TiC, TiN, WC, Mo2C, Co and Ni; the wet grinding medium adopts absolute ethyl alcohol, and the addition amount of the absolute ethyl alcohol is that all the main material powder and the grinding balls can be immersed; the grinding ball is made of hard alloy;
② drying the slurry obtained in step ① in a vacuum oven with vacuum degree of 70Pa and drying temperature of 80 ℃ for 3.5-4.5h to obtain uniformly dried mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 30-50 ℃ to keep the binder not to be separated out, starting low speed stirring, the stirring direction is clockwise, the stirring speed is 30-50 r/min, simultaneously adding alcohol in a uniform speed spraying mode, stopping adding alcohol and stirring after 10min, taking out the powder, pouring the powder into a 80-mesh screen, applying 2-8N pressure to knead the powder until all the powder passes through the screen, then slowly pouring the sieved powder into a 100-mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100-mesh screen is granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen to obtain the granulated TiC-based cermet powder for standby, if the amount of the fine powder passing through the 100-mesh screen is more (>30g), continuously repeating step ① on the difference screen to granulate, and if the amount of the fine powder is less, discarding;
③, placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying, wherein the drying temperature is 50 ℃, the vacuum degree is 50Pa-100Pa during drying, and the drying time is 5h-7h, so as to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace for removing a binder, and specifically comprising the following steps of:
① loose placing the dried and granulated TiC-based cermet powder prepared in step (2) in a corundum boat, covering a temperature equalizing cover, placing in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to below 0.01Pa, heating from room temperature to 200 ℃ at the heating rate of 6 ℃/min, and then keeping the temperature for 1.5 h;
② continuously heating to 650 deg.C at a heating rate of 4 deg.C/min, and keeping the temperature for 4.5 h;
③ cooling to room temperature to obtain TiC-based cermet powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method to obtain presintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method comprises the following specific steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 500 ℃ at the heating rate of 8 ℃/min, and then preserving heat for 1 h;
② heating to 700 deg.C at a heating rate of 4 deg.C/min, and maintaining for 2 h;
③ heating to 1100 deg.C at a heating rate of 4 deg.C/min, and holding for 4 hr;
④ and cooling in furnace to obtain the pre-sintered alloyed titanium carbide-based cermet thermal spraying powder.
Example 7:
the method comprises the following steps:
wet grinding in the step (1), differential screening granulation in the step (2) and vacuum degreasing in the step (3) are the same as in the example 1;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a rapid sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method specifically comprises the following steps:
placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a corundum boat, placing the corundum boat into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying a direct-current electric field strength of 20V/cm to the granulated TiC-based metal ceramic powder, simultaneously heating the granulated TiC-based metal ceramic powder at a heating rate of 10 ℃/min, and when the temperature is increased to 950 ℃, enabling particles to have strong reaction so as to be instantly densified, and stopping applying current and heating; finally, the titanium carbide-based cermet thermal spraying powder which is presintered and alloyed is obtained by furnace cooling.
Example 8:
the method comprises the following steps:
wet grinding in the step (1), differential screening granulation in the step (2) and vacuum degreasing in the step (3) are the same as in the example 1;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a rapid sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method specifically comprises the following steps:
placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a corundum boat, placing the corundum boat into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying a direct-current electric field strength of 35V/cm to the granulated TiC-based metal ceramic powder, simultaneously heating the granulated TiC-based metal ceramic powder at a heating rate of 8 ℃/min, and when the temperature is increased to 900 ℃, carrying out a strong reaction on particles so as to carry out instant densification, and stopping applying current and heating; finally, the titanium carbide-based cermet thermal spraying powder which is presintered and alloyed is obtained by furnace cooling.
Example 9:
the method comprises the following steps:
wet grinding in the step (1), differential screening granulation in the step (2) and vacuum degreasing in the step (3) are the same as in the example 1;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a rapid sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder. The method specifically comprises the following steps:
placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a corundum boat, placing the corundum boat into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying a direct-current electric field strength of 30V/cm to the granulated TiC-based metal ceramic powder, simultaneously heating the granulated TiC-based metal ceramic powder at a heating rate of 12 ℃/min, and when the temperature is increased to 920 ℃, carrying out a strong reaction on particles so as to carry out instant densification, and stopping applying current and heating; finally, the titanium carbide-based cermet thermal spraying powder which is presintered and alloyed is obtained by furnace cooling.
Second, Experimental example
The titanium carbide-based cermet thermal spraying powders prepared in examples 1 to 9 are respectively sprayed on the surface of a steel substrate through a laser cladding process to form a coating, and examples 1 to 9 respectively correspond to a sample 1, a sample 2, a sample 3, a sample 4, a sample 5, a sample 6, a sample 7, a sample 8 and a sample 9; the coating thickness of sample 1, sample 2, sample 3, sample 4, sample 5, sample 6, sample 7, sample 8 and sample 9 was 1.2 mm;
comparative example 1 is: the WC-Co coating is formed on the surface of the steel substrate by spraying through a laser cladding process, and the thickness of the WC-Co coating is 1.8 mm; reference is made to comparative sample 1;
comparative example 2 is: cr formed on the surface of a steel substrate by spraying through a laser cladding process3C2Coating of Cr3C2The thickness of the coating is 2.5 mm; this is designated as comparative sample 2.
Samples 1, 2, 3, 4, 5, 6, 7, 8, 9 were tested for corrosion resistance, oxidation resistance, hardness and wear resistance with comparative sample 1 and comparative sample 2 of the comparative example, the results of which are shown in table 3 below:
the test method comprises the following steps:
1. corrosion resistance:
the weight loss was measured by the immersion corrosion test by subjecting all samples to H at 1 mol/L2SO4Soaking in the solution for 4 days, and testing the weight and surface area of the sample before corrosion and the weight after corrosion to obtain the corrosion rate (g/cm)2)；
2. Oxidation resistance:
measured by measuring the weight gain of all samples before and after oxidation after high temperature oxidation (800 ℃) for 40h in static air, the unit of the obtained oxidation rate is g/cm2；
3. Hardness:
measured with a vickers hardness tester, in HV;
4. wear resistance:
the wear resistance of the coating is characterized by loading all the samples on a reciprocating friction-wear machine respectively for 50N, wearing time for 10min and measuring the depth of the grinding marks, and the unit is mum.
Table 3 results of performance testing
| Corrosion resistance, g/cm2 | Oxidative weight gain, g/cm2 | Hardness, HV | Depth of grinding mark, μm | |
| Comparative sample 1 | 0.043 | 1.2 | 1400 | 62 |
| Comparative sample 2 | 0.012 | 0.72 | 1050 | 84 |
| Sample No. 1 | 0.007 | 0.11 | 1430 | 27 |
| Sample No. 2 | 0.016 | 0.20 | 1370 | 47 |
| Sample No. 3 | 0.007 | 0.45 | 1390 | 45 |
| Sample No. 4 | 0.010 | 0.60 | 1440 | 23 |
| Sample No. 5 | 0.015 | 0.33 | 1510 | 18 |
| Sample No. 6 | 0.013 | 0.56 | 1280 | 58 |
| Sample 7 | 0.012 | 0.60 | 1260 | 60 |
| Sample 8 | 0.011 | 0.30 | 1510 | 20 |
| Sample 9 | 0.011 | 0.38 | 1360 | 49 |
WC-Co coating and Cr3C2And (4) coating.
The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and all the changes or substitutions should be covered within the scope of the present invention.
Claims (10)
1. A titanium carbide-based cermet thermal spray powder is characterized in that: the preparation method comprises the following main materials in percentage by weight:
TiC 20%-40%；
TiN 20%-30%；
WC 10%-20%；
Mo2C 2%-6%；
Co 10%-30%；
Ni 10%-30%；
the sum of the weight percentages of the main materials is 100 percent.
2. The titanium carbide-based cermet thermal spray powder of claim 1, wherein: the weight percentages of the main materials are respectively as follows:
TiC 25%-35%；
TiN 20%-25%；
WC 12%-18%；
Mo2C 3%-5%；
Co 15%-25%；
Ni 15%-25%；
the sum of the weight percentages of the main materials is 100 percent.
3. The titanium carbide-based cermet thermal spray powder of claim 2, wherein: the weight percentages of the main materials are respectively as follows:
TiC 32%；
TiN 22%；
WC 12%；
Mo2C 4%；
Co 15%；
Ni 15%。
4. the titanium carbide-based cermet thermal spray powder of any one of claims 1-3, wherein: the preparation method also comprises auxiliary materials, wherein the auxiliary materials comprise a binder and a wet grinding medium, and the addition amount of the binder is 3-6% of the total weight of the main materials.
5. The method for preparing titanium carbide-based cermet thermal spray powder as defined in any one of claims 1 to 4, wherein: the method comprises the following steps:
(1) wet grinding:
① mixing TiC, TiN, WC and Mo2C. Adding Co and Ni into a ball milling tank according to a ratio, adding a bonding agent and a wet milling medium, and carrying out wet milling to obtain uniformly mixed slurry;
② drying the slurry obtained in step ① to obtain a dry and uniform mixed powder;
(2) and (3) differential screening granulation:
① placing the mixed powder obtained in step (1) into a constant temperature stirrer vessel, keeping the temperature at 30-50 deg.C, starting low speed stirring, simultaneously adding alcohol in form of uniform spraying, stopping adding alcohol and stirring after 10min, taking out the powder and pouring into a 80 mesh screen, applying pressure to knead the powder until all the powder passes through the screen, slowly pouring the sieved powder into a 100 mesh screen, vibrating the screen to allow fine powder to automatically pass through the screen, wherein the powder which does not pass through the 100 mesh screen is the granulated TiC-based cermet powder, and keeping for later use;
②, continuously repeating step ① on the fine powder passing through the screen mesh to continuously obtain the granulated TiC-based metal ceramic powder for later use;
③ placing the granulated TiC-based metal ceramic powder into a vacuum oven for low-temperature drying to obtain dried granulated TiC-based metal ceramic powder;
(3) vacuum degreasing:
placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace to remove a binder, so as to obtain granulated TiC-based metal ceramic powder;
(4) powder sintering:
and (4) sintering the granulated TiC-based metal ceramic powder prepared in the step (3) by a slow sintering method or a fast sintering method to obtain pre-sintered alloyed titanium carbide-based metal ceramic thermal spraying powder.
6. The method of preparing titanium carbide-based cermet thermal spray powder as defined in claim 5, wherein: in the step (3), the vacuum degreasing comprises the following steps:
①, placing the dried and granulated TiC-based metal ceramic powder prepared in the step (2) in a vacuum degreasing furnace, after the vacuum degree in the furnace is pumped to be below 0.01Pa, heating the powder from room temperature to 200-300 ℃ at the heating rate of 4-6 ℃/min, and then keeping the temperature for 1.5-2.5 h;
② continuously heating to 550-650 deg.C at a heating rate of 4-6 deg.C/min, and keeping the temperature for 4.5-5.5 h;
③ and finally cooling to room temperature along with the furnace to obtain the granular TiC-based metal ceramic powder.
7. The method of preparing titanium carbide-based cermet thermal spray powder as defined in claim 6, wherein: in the step (4), the slow sintering method includes the following steps:
①, placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, sintering under the protection of nitrogen, firstly heating to 500-600 ℃ at the heating rate of 8-12 ℃/min, and then preserving heat for 1-2 h;
② is heated to 700-800 ℃ at the heating rate of 4-6 ℃/min, and then the temperature is kept for 1-2 h;
③ heating to 1100-1200 deg.C at a heating rate of 4-6 deg.C/min, and holding for 2-4 h;
④ cooling with furnace to obtain pre-sintered alloyed titanium carbide-based cermet thermal spraying powder;
the rapid sintering method comprises the following steps: placing the granulated TiC-based metal ceramic powder prepared in the step (3) into a vacuum atmosphere furnace, inserting two platinum wires into two ends of the granulated TiC-based metal ceramic powder, applying current to the granulated TiC-based metal ceramic powder, simultaneously heating the temperature in the furnace at the heating rate of 8-12 ℃/min, and stopping applying the current and heating when the temperature is raised to 850-950 ℃; finally, the titanium carbide-based cermet thermal spraying powder which is presintered and alloyed is obtained by furnace cooling.
8. The method for preparing titanium carbide-based cermet thermal spray powder as defined in any one of claims 5 to 7, wherein: in the step (1), the added adhesive is paraffin or polyethylene glycol, and the adding amount of the adhesive is 3% -6% of the total weight of the main materials.
9. The method of preparing titanium carbide-based cermet thermal spray powder of claim 8 wherein: in the step (1), during wet grinding, the material of the grinding ball is hard alloy, and the wet grinding rotating speed is 60r/min-100 r/min.
10. The method of preparing titanium carbide-based cermet thermal spray powder of claim 9, wherein: in the step (2), the applied pressure is 2N-8N when the mixture is sieved by an 80-mesh sieve.
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| CN114000085A (en) * | 2021-09-17 | 2022-02-01 | 崇义章源钨业股份有限公司 | Titanium carbonitride-based thermal spraying powder and preparation method and application thereof |
| CN114000085B (en) * | 2021-09-17 | 2023-06-02 | 崇义章源钨业股份有限公司 | Titanium carbonitride-based thermal spraying powder and preparation method and application thereof |
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