Metal ceramic spraying powder and preparation method thereof

Abstract

The invention discloses metal ceramic spraying powder and a preparation method thereof, and relates to the technical field of metal ceramic powder spraying materials. The metal ceramic spraying powder comprises one or more of titanium carbonitride, titanium carbide and titanium nitride; the metal ceramic spraying powder disclosed by the invention is uniform in component and has excellent sphericity, so that the spraying powder is good in flowability, and an obtained coating is good in stability; the coating formed by the spraying powder and the matrix metal surface layer is high in binding force, the advantages of corrosion resistance, high temperature resistance, low porosity, high density, high red hardness and the like are also achieved, and the preparation method is simple, easy to implement, low in cost and easy for mass production.

Description

Technical Field

[0001] The present application relates to the technical field of metal ceramic powder spraying materials, and in particular to metal ceramic spraying powder and a preparation method thereof. Background Art

[0002] In recent years, mining, metallurgy, cement and other industries have developed towards large-scale development. In the fields of building materials, thermal power generation, metallurgical mining and equipment manufacturing, the direct economic losses caused by product failure due to wear and tear at home and abroad have reached tens of billions or even more than 100 billion yuan each year. Among them, the wear-resistant materials that consume abrasive wear alone reach millions of tons of metal each year, and are still growing at a rate of 15% per year. According to incomplete statistics from my country's metallurgical, coal, power and other industries, metal wear is one of the main causes of mechanical parts failure in metal parts operating in the environment of sediment, dust, ore and other media. The loss is very alarming. The weight of metal materials worn out each year is more than 3 million tons, and the loss is as high as tens of billions of yuan. Data show that nearly one-third of the world's primary energy is lost due to wear and tear.

[0003] Thermal spraying technology utilizes various heat sources to melt the materials to be sprayed (generally corrosion-resistant metals, alloys, ceramics, plastics, and other corrosion-resistant composite materials) into a molten state, and then uses airflow to atomize the materials at high speed to form a "particle mist flow" that is deposited on the surface of the pretreated workpiece to form a deposited coating that is tightly bonded to the body, thereby protecting the body.

[0004] In recent years, thermal spraying technology has been continuously improved, and equipment, materials and processes have been rapidly developed. Although thermal spraying has advantages such as fast deposition speed, high productivity and wide adaptability, thermal spray coatings have high porosity, poor wear resistance and corrosion resistance, uneven coating structure, and poor bonding strength between coating and substrate, which seriously affects the performance of the coating. Summary of the invention

[0005] In view of this, the present application provides metal ceramic spray powder and its preparation method, aiming to improve the existing thermal spray coatings with high porosity, poor wear resistance and corrosion resistance, uneven coating structure, and poor bonding strength between the coating and the substrate, which seriously affects the performance of the coating.

[0006] The embodiment of the present application is implemented in that the metal ceramic spraying powder includes one or more of titanium carbonitride, titanium carbide and titanium nitride.

[0007] Optionally, in some embodiments of the present application, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium carbonitride, 0% to 50% titanium carbide, and 0% to 50% titanium nitride; titanium carbonitride is the main phase, and titanium carbide and / or titanium nitride are the auxiliary phases.

[0008] Optionally, in some embodiments of the present application, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium carbide, 0% to 50% titanium carbonitride, and 0% to 50% titanium nitride; titanium carbide is the main phase, and titanium carbonitride and / or titanium nitride are auxiliary phases.

[0009] Optionally, in some embodiments of the present application, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium nitride, 0% to 50% titanium carbonitride, and 0% to 50% titanium carbide; titanium nitride is the main phase, and titanium carbonitride and / or titanium carbide are auxiliary phases.

[0010] Optionally, in some embodiments of the present application, the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is not greater than 4.0 microns; and / or

[0011] The titanium carbide is in the form of a powder, the titanium carbide powder having a Fsss particle size of not greater than 4.0 microns; and / or

[0012] The titanium nitride is in the form of powder, and the Fsss particle size of the titanium nitride powder is not greater than 4.0 microns.

[0013] Accordingly, the present application also provides a method for preparing a metal ceramic spray powder, comprising:

[0014] Providing a mixed slurry, the mixed slurry comprising one or more of titanium carbonitride, titanium carbide and titanium nitride;

[0015] Spray granulate the mixed slurry to obtain pre-solidified precursor powder;

[0016] The pre-solid solution precursor powder is subjected to a heating and degreasing stage, a vacuum sintering stage and a cooling stage in sequence to obtain a metal ceramic block;

[0017] The metal ceramic spray powder is obtained by crushing and screening.

[0018] Optionally, in some embodiments of the present application, one or more of titanium carbonitride, titanium carbide and titanium nitride are weighed according to the above mass percentage to obtain a raw material powder, a dispersant and a molding agent are added to the raw material powder, and the prepared raw material is obtained after mixing evenly, and a mixed slurry is obtained by wet grinding; and / or

[0019] The mixed slurry is placed in a spray tower for spray spheroidization granulation, the inlet temperature of the spray tower is T1, the outlet temperature is T2, the centrifugal atomization speed of the spray spheroidization granulation is v1, and the frequency is f; and / or

[0020] The heating and degreasing stage is carried out according to the preheating, vacuuming, heating and insulation procedures, preheating to T3 temperature, the heating rate does not exceed v2, the insulation time is t1, vacuuming to below P, heating to T4, the heating rate does not exceed v3, and at T4 temperature, insulation time t2; and / or

[0021] During the vacuum sintering stage, the heating rate does not exceed v4, the heating temperature rises from T4 to T5, and is kept warm for t3 time; the heating rate does not exceed v5, when the sintering temperature reaches T6, it is kept warm for t4 time; the heating rate does not exceed v6, when the sintering temperature reaches T7, it is kept warm for t5 time.

[0022] Optionally, in some embodiments of the present application, the prepared raw materials are added into a grinding carbide or stainless steel ball mill of a ball mill, and a solvent is added and ball milled to obtain a mixed slurry; and / or

[0023] T1 is 180°C to 280°C; and / or

[0024] T2 is 100°C to 130°C; and / or

[0025] v1 is 5500 rpm to 9500 rpm; and / or

[0026] f is between 85 Hz and 180 Hz; and / or

[0027] T3 is 80°C to 200°C; and / or

[0028] v2 does not exceed 10℃ / min; and / or

[0029] t1 is 30 min to 60 min; and / or

[0030] P is less than 10Pa; and / or

[0031] T4 is 280°C to 450°C; and / or

[0032] v3 does not exceed 5℃ / min; and / or

[0033] t2 is 50 min to 120 min; and / or

[0034] v4 does not exceed 5℃ / min; and / or

[0035] T5 is 520°C to 600°C; and / or

[0036] t3 is 10 min to 90 min; and / or

[0037] v5 does not exceed 4℃ / min; and / or

[0038] T6 is 900°C to 1150°C; and / or

[0039] t4 is 50 min to 150 min; and / or

[0040] v6 does not exceed 4℃ / min; and / or

[0041] T7 is 1150°C to 1350°C; and / or

[0042] t5 is 30min~120min.

[0043] Optionally, in some embodiments of the present application, the dispersant includes one or more of dodecylbenzenesulfonic acid, stearic acid and oleic acid; and / or

[0044] The molding agent is one or more of rubber, paraffin and PEG; and / or

[0045] The solvent includes one or more of gasoline, ethylene glycol and hexane.

[0046] Optionally, in some embodiments of the present application, in the mixed slurry, the ratio of solid to liquid is (5-7): (5-3); and / or

[0047] The mass fraction of the dispersant to the total amount of the raw material powder is 0.1% to 0.5%; and / or

[0048] The mass fraction of the molding agent to the total amount of raw material powder is 2.5% to 4.5%; and / or

[0049] The volume mass ratio of the solvent to the total amount of the raw material powder is 280ml / Kg to 500ml / Kg; and / or

[0050] During ball milling, 85% to 90% of the total volume of the solvent is first added, and the remaining solvent is added 8 to 10 hours before the end of ball milling; and / or

[0051] The ball mill is a rolling ball mill or a vertical stirring ball mill, the diameter of the carbide balls is 6.25 mm to 12 mm, the ball-to-material ratio is 2.5:1 to 10:1, the ball milling speed is 68 to 85 rpm, and the ball milling time is 16 h to 90 h.

[0052] In the present application, PEG is polyethylene glycol.

[0053] The metal ceramic spray powder of the present application has uniform composition and excellent sphericity, so the spray powder has good fluidity and the obtained coating has good stability; the coating formed by the spray powder and the surface layer of the base metal has strong bonding force, and also has the advantages of excellent comprehensive performance such as corrosion resistance, high temperature resistance, low porosity, high density, and high red hardness;

[0054] In the preparation method of the present application, the purpose of using multi-stage sintering in the heating and degreasing stage is to ensure that the forming agent, dispersant, etc. can be completely eliminated and the purity of the powder components can be ensured; the purpose of using multi-stage sintering in the vacuum sintering stage is to ensure uniform degreasing of the powder, solidify the morphology, and ensure the roundness and uniformity of the spherical powder components; the purpose of controlling the heating rate is to effectively remove the forming agent, dispersant, etc., and in addition, it can prevent the spheres from breaking due to excessively fast heating of the powder. The entire preparation method is simple, easy to operate, low-cost, and easy to mass produce. BRIEF DESCRIPTION OF THE DRAWINGS

[0055] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For those skilled in the art, other drawings can be obtained based on these drawings without paying any creative work.

[0056] Figure 1 It is a flow chart of the method for preparing metal ceramic spray powder provided in the embodiment of the present application;

[0057] Figure 2 is a scanning electron microscope image provided in Example 1 of the present application;

[0058] Figure 3 is a scanning electron microscope image provided in Example 2 of the present application;

[0059] Figure 4 is a scanning electron microscope image provided in Example 7 of the present application;

[0060] Figure 5 is a scanning electron microscope image provided in Example 10 of the present application;

[0061] Figure 6 This is a scanning electron microscope image provided in Example 18 of the present application. DETAILED DESCRIPTION

[0062] The technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without making creative work belong to the scope of protection of the present application. In addition, it should be understood that the specific implementation methods described herein are only used to illustrate and explain the present application, and are not used to limit the present application.

[0063] In this application, further, in the description of this application, the term "including" means "including but not limited to." The terms first, second, third, etc. are used merely as labels and do not impose numerical requirements or establish a sequence.

[0064] In this application, "and / or" describes the association relationship of associated objects, indicating that there may be three relationships. For example, A and / or B can represent: A exists alone, A and B exist at the same time, and B exists alone. A and B can be singular or plural.

[0065] In the present application, "at least one" means one or more, and "plurality" means two or more. "One or several", "at least one of the following" or similar expressions refer to any combination of these items, including any combination of single items or plural items. For example, "at least one of a, b, or c", or "at least one of a, b, and c" can all mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, c can be single or multiple, respectively.

[0066] Various embodiments of the present application may be presented in the form of a range; it should be understood that the description in the form of a range is only for convenience and brevity, and should not be understood as a rigid limitation on the scope of the present application; therefore, the range description should be considered to have specifically disclosed all possible sub-ranges and single numerical values ​​within the range. For example, the range description from 1 to 6 should be considered to have specifically disclosed sub-ranges, such as from 1 to 3, from 1 to 4, from 1 to 5, from 2 to 4, from 2 to 6, from 3 to 6, etc., as well as single numbers within the range, such as 1, 2, 3, 4, 5 and 6, which apply regardless of the range. In addition, whenever a numerical range is indicated herein, it is meant to include any cited number (fractional or integer) within the indicated range.

[0067] The technical solution of this application is as follows:

[0068] In a first aspect, an embodiment of the present application provides a metal ceramic spray powder, including one or more of titanium carbonitride, titanium carbide and titanium nitride.

[0069] The metal ceramic spray powder of the present application has uniform composition and excellent sphericity, so its spray powder has good fluidity and the obtained coating has good stability; the coating formed by the spray powder and the surface layer of the base metal has strong bonding force, and also has the advantages of excellent comprehensive performance such as corrosion resistance, high temperature resistance, low porosity, high density, and high red hardness. The surface deposition layer formed after spraying has strong corrosion resistance and hardness; in the preparation method of the present application, the purpose of using multi-stage sintering in the heating and degreasing stage is to ensure that the forming agent, dispersant, etc. can be completely eliminated to ensure the purity of the powder composition; the purpose of using multi-stage sintering in the vacuum sintering stage is to ensure uniform degreasing of the powder, solidification morphology, and roundness and uniformity of the composition of the spherical powder; the purpose of controlling the heating rate is to effectively remove the forming agent, dispersant, etc., and in addition, it can prevent the sphere from breaking due to excessively fast heating of the powder. The entire preparation method is simple and easy to implement, low cost and easy to mass produce.

[0070] Further, the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is not greater than 4.0 microns, for example, it can be 0.1 microns, 0.2 microns, 0.5 microns, 0.8 microns, 1 micron, 1.2 microns, 1.4 microns, 1.6 microns, 1.8 microns, 2 microns, 2.2 microns, 2.5 microns, 2.8 microns, 3 microns, 3.1 microns, 3.2 microns, 3.5 microns, 3.6 microns, 3.8 microns, 4 microns, etc. The wear resistance and matrix bonding strength are increased within the micron range.

[0071] Further, the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is not greater than 4.0 microns, for example, it can be 0.1 micron, 0.2 micron, 0.5 micron, 0.8 micron, 1 micron, 1.2 micron, 1.4 micron, 1.6 micron, 1.8 micron, 2 micron, 2.2 micron, 2.5 micron, 2.8 micron, 3 micron, 3.1 micron, 3.2 micron, 3.5 micron, 3.6 micron, 3.8 micron, 4 micron, etc. Wear resistance and matrix bonding strength are increased within the micron range.

[0072] Further, the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is not greater than 4.0 microns, for example, it can be 0.1 micron, 0.2 micron, 0.5 micron, 0.8 micron, 1 micron, 1.2 micron, 1.4 micron, 1.6 micron, 1.8 micron, 2 micron, 2.2 micron, 2.5 micron, 2.8 micron, 3 micron, 3.1 micron, 3.2 micron, 3.5 micron, 3.6 micron, 3.8 micron, 4 micron, etc. Wear resistance and matrix bonding strength are increased within the micron range.

[0073] In some embodiments, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium carbonitride, 0% to 50% titanium carbide, and 0% to 50% titanium nitride.

[0074] Further, by mass percentage, the metal ceramic spray powder includes 50% to 100% titanium carbonitride, preferably 55% to 95% titanium carbonitride, more preferably 60% to 90% titanium carbonitride, more preferably 65% ​​to 85% titanium carbonitride, more preferably 70% to 80% titanium carbonitride; 0% to 50% titanium carbide, preferably 5% to 45% titanium carbide, more preferably 10% to 40% titanium carbide, more preferably 15% to 35% titanium carbide, more preferably 20% to 30% titanium carbide; 0% to 50% titanium nitride, preferably 5% to 45% titanium nitride, more preferably 10% to 40% titanium nitride, more preferably 15% to 35% titanium nitride, more preferably 20% to 30% titanium nitride.

[0075] Furthermore, in the metal ceramic spray powder, when the content of titanium carbonitride is greater than 50% and less than 100%, the content of titanium carbide is greater than 0% and less than 50%, and the content of titanium nitride is 0%, measured by mass percentage; titanium carbonitride is the main phase and titanium carbide is the auxiliary phase.

[0076] Furthermore, in the metal ceramic spray powder, when the content of titanium carbonitride is greater than 50% and less than 100%, the content of titanium nitride is greater than 0% and less than 50%, and the content of titanium carbide is 0% by mass percentage; titanium carbonitride is the main phase and titanium nitride is the auxiliary phase.

[0077] Furthermore, in the metal ceramic spray powder, when the content of titanium carbonitride is greater than 50% and less than 100%, the content of titanium carbide is greater than 0% and less than 50%, and the content of titanium nitride is greater than 0% and less than 50%, measured by mass percentage; titanium carbonitride is the main phase, and titanium carbide and titanium nitride are auxiliary phases.

[0078] In some embodiments, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium carbide, 0% to 50% titanium carbonitride, and 0% to 50% titanium nitride.

[0079] Further, by mass percentage, the metal ceramic spray powder includes 50% to 100% titanium carbide, preferably 55% to 95% titanium carbide, more preferably 60% to 90% titanium carbide, more preferably 65% ​​to 85% titanium carbide, more preferably 70% to 80% titanium carbide; 0% to 50% titanium carbonitride, preferably 5% to 45% titanium carbonitride, more preferably 10% to 40% titanium carbonitride, more preferably 15% to 35% titanium carbonitride, more preferably 20% to 30% titanium carbonitride; 0% to 50% titanium nitride, preferably 5% to 45% titanium nitride, more preferably 10% to 40% titanium nitride, more preferably 15% to 35% titanium nitride, more preferably 20% to 30% titanium nitride.

[0080] Furthermore, in the metal ceramic spray powder, by mass percentage, when the content of titanium carbide is greater than 50% and less than 100%, the content of titanium carbonitride is greater than 0% and less than 50%, and the content of titanium nitride is 0%; titanium carbide is the main phase and titanium carbonitride is the auxiliary phase.

[0081] Furthermore, in the metal ceramic spray powder, by mass percentage, when the content of titanium carbide is greater than 50% and less than 100%, the content of titanium nitride is greater than 0% and less than 50%, and the content of titanium carbonitride is 0%; titanium carbide is the main phase and titanium nitride is the auxiliary phase.

[0082] Furthermore, in the metal ceramic spray powder, when the content of titanium carbide is greater than 50% and less than 100%, the content of titanium carbonitride is greater than 0% and less than 50%, and the content of titanium nitride is greater than 0% and less than 50%, measured by mass percentage; titanium carbide is the main phase, and titanium carbonitride and titanium nitride are auxiliary phases.

[0083] In some embodiments, the metal ceramic spray powder includes, by mass percentage, 50% to 100% titanium nitride, 0% to 50% titanium carbonitride, and 0% to 50% titanium carbide.

[0084] Further, by mass percentage, the metal ceramic spray powder includes 50% to 100% titanium nitride, preferably 55% to 95% titanium nitride, more preferably 60% to 90% titanium nitride, more preferably 65% ​​to 85% titanium nitride, more preferably 70% to 80% titanium nitride; 0% to 50% titanium carbonitride, preferably 5% to 45% titanium carbonitride, more preferably 10% to 40% titanium carbonitride, more preferably 15% to 35% titanium carbonitride, more preferably 20% to 30% titanium carbonitride; 0% to 50% titanium carbide, preferably 5% to 45% titanium carbide, more preferably 10% to 40% titanium carbide, more preferably 15% to 35% titanium carbide, more preferably 20% to 30% titanium carbide.

[0085] Furthermore, in the metal ceramic spray powder, by mass percentage, when the content of titanium nitride is greater than 50% and less than 100%, the content of titanium carbonitride is greater than 0% and less than 50%, and the content of titanium carbide is 0%; titanium nitride is the main phase and titanium carbonitride is the auxiliary phase.

[0086] Furthermore, in the metal ceramic spray powder, by mass percentage, when the content of titanium nitride is greater than 50% and less than 100%, the content of titanium carbide is greater than 0% and less than 50%, and the content of titanium carbonitride is 0%; titanium nitride is the main phase and titanium carbide is the auxiliary phase.

[0087] Furthermore, in the metal ceramic spray powder, when the content of titanium nitride is greater than 50% and less than 100%, the content of titanium carbonitride is greater than 0% and less than 50%, and the content of titanium carbide is greater than 0% and less than 50%, measured by mass percentage; titanium nitride is the main phase, and titanium carbonitride and titanium carbide are auxiliary phases.

[0088] See also Figure 1 In a second aspect, the present application provides a method for preparing a metal ceramic spray powder, comprising:

[0089] S01. providing a mixed slurry, wherein the mixed slurry comprises one or more of titanium carbonitride, titanium carbide and titanium nitride;

[0090] S02, spraying and granulating the mixed slurry to obtain a pre-solidified precursor powder;

[0091] S03, sequentially performing a heating and degreasing stage, a vacuum sintering stage, and a cooling stage on the pre-solid solution precursor powder to obtain a metal ceramic block;

[0092] S04, crushing and screening to obtain metal ceramic spray powder.

[0093] In the S01:

[0094] In some embodiments, one or more of titanium carbonitride, titanium carbide and titanium nitride are weighed according to the above mass percentage to obtain a raw material powder.

[0095] It is understandable that when the raw material powder is any one of titanium carbonitride, titanium carbide or titanium nitride, mixing is not required. It is also understandable that when two or three of titanium carbonitride, titanium carbide and titanium nitride are used, mixing is required after weighing.

[0096] Furthermore, a dispersant and a molding agent are added to the raw material powder, mixed evenly to obtain a prepared raw material, and wet-grinded to obtain a mixed slurry.

[0097] Furthermore, the dispersant includes one or more of dodecylbenzenesulfonic acid, stearic acid and oleic acid.

[0098] Furthermore, the mass fraction of the dispersant to the total amount of raw material powder is 0.1% to 0.5%, for example, it can be 0.1%, 0.15%, 0.2%, 0.25%, 0.3%, 0.35%, 0.4%, 0.45%, 0.5%, etc.

[0099] Furthermore, the molding agent is one or more of rubber, paraffin and PEG.

[0100] Furthermore, the mass fraction of the molding agent to the total amount of the raw material powder is 2.5% to 4.5%, for example, it can be 2.5%, 3%, 3.5%, 4%, 4.5%, etc.

[0101] Furthermore, the prepared raw materials are added into a grinding carbide or stainless steel ball mill of a ball mill, and a solvent is added and ball milling is performed to obtain a mixed slurry.

[0102] Furthermore, in the mixed slurry, the ratio of solid to liquid is (5-7):(5-3), for example, 5:5, 5.2:4.8, 5.5:4.5, 5.8:4.2, 6:4, 6.2:3.8, 6.5:3.5, 6.8:3.2, 7:3, etc. Within the ratio range, the sphericity of the preparation is guaranteed.

[0103] It will be appreciated that the ratio of solid to liquid is a mass ratio.

[0104] It can be understood that the solid is the raw material powder and the liquid is the ball milling medium.

[0105] Furthermore, the volume mass ratio of the solvent to the total amount of raw material powder is 280ml / Kg to 500ml / Kg, for example, it can be 280ml / Kg, 300ml / Kg, 320ml / Kg, 350ml / Kg, 380ml / Kg, 400ml / Kg, 420ml / Kg, 450ml / Kg, 480ml / Kg, 500ml / Kg, etc.

[0106] Furthermore, during ball milling, 85% to 90% of the total volume of the solvent is first added, for example, 85%, 86%, 87%, 88%, 89%, 90%, etc., and the remaining solvent is added 8h to 10h before the end of ball milling, for example, 8h, 8.5h, 9h, 9.5h, 10h, etc.

[0107] Furthermore, the solvent includes one or more of gasoline, ethylene glycol and hexane.

[0108] Furthermore, the ball mill is a rolling ball mill or a vertical stirring ball mill, the ball diameter of the cemented carbide ball is 6.25mm-12mm, for example, it can be 6.5mm, 7mm, 7.5mm, 8mm, 8.5mm, 9mm, 9.5mm, 10mm, 10.5mm, 11mm, 11.5mm, 12mm, etc.; the ball-to-material ratio is 2.5:1-10:1, for example, it can be 2.5:1, 3:1, 3.5:1, 4:1, 4.5:1, 5:1, 5.5:1, 6:1, 6.5:1, 7:1, 7.5:1, 8:1 , 8.5:1, 9:1, 9.5:1, 10:1; the ball milling speed is 68-85 rpm, for example, it can be 68 rpm, 70 rpm, 72 rpm, 75 rpm, 78 rpm, 79 rpm, 80 rpm, 82 rpm, 84 rpm, 85 rpm, etc.; the ball milling time is 16h-90h, for example, it can be 16h, 20h, 25h, 30h, 35h, 40h, 45h, 50h, 55h, 60h, 65h, 70h, 75h, 80h, 85h, 90h, etc.

[0109] In the S02:

[0110] In some embodiments, the mixed slurry is placed in a spray tower for spray spheroidization granulation.

[0111] Furthermore, the pre-solid solution precursor powder is spherical.

[0112] Furthermore, the inlet temperature in the spray tower is T1, the outlet temperature is T2, the centrifugal atomization speed of the spray spheroidization granulation is v1, and the frequency is f.

[0113] Furthermore, T1 is 180°C to 280°C, for example, 180°C, 190°C, 200°C, 210°C, 220°C, 230°C, 240°C, 250°C, 260°C, 270°C, 280°C, etc.

[0114] Further, T2 is 100°C to 130°C, for example, it can be 100°C, 102°C, 105°C, 108°C, 110°C, 112°C, 115°C, 118°C, 120°C, 122°C, 125°C, 128°C, 130°C, etc.

[0115] Furthermore, v1 is 5500 rpm to 9500 rpm, for example, 5500 rpm, 6000 rpm, 6500 rpm, 7000 rpm, 7500 rpm, 8000 rpm, 8500 rpm, 9000 rpm, 9500 rpm, etc.

[0116] Furthermore, f is 85 Hz to 180 Hz, for example, it can be 85 Hz, 90 Hz, 95 Hz, 100 Hz, 105 Hz, 110 Hz, 115 Hz, 120 Hz, 125 Hz, 130 Hz, 135 Hz, 140 Hz, 145 Hz, 150 Hz, 155 Hz, 160 Hz, 165 Hz, 170 Hz, 175 Hz, 180 Hz, etc.

[0117] In said S03:

[0118] In some embodiments, the heating and degreasing stage is carried out according to the preheating, vacuuming, heating and insulation processes, preheating to T3 temperature, the heating rate does not exceed v2, the insulation time is t1, vacuuming to below P, heating to T4, the heating rate does not exceed v3, and insulation at T4 for t2.

[0119] Furthermore, T3 is 80°C to 200°C, for example, it can be 80°C, 90°C, 100°C, 110°C, 120°C, 130°C, 140°C, 150°C, 160°C, 170°C, 180°C, 190°C, 200°C, etc.

[0120] v2 does not exceed 10℃ / min, for example, it may be no more than 0.5℃ / min, no more than 1℃ / min, no more than 2℃ / min, no more than 3℃ / min, no more than 4℃ / min, no more than 5℃ / min, no more than 6℃ / min, no more than 7℃ / min, no more than 8℃ / min, no more than 9℃ / min, no more than 10℃ / min, etc.

[0121] t1 is 30 min to 60 min, for example, it can be 30 min, 35 min, 40 min, 45 min, 50 min, 55 min, 60 min, etc.

[0122] P is 10 Pa or less, for example, it may be 1 Pa or less, 2 Pa or less, 3 Pa or less, 4 Pa ​​or less, 5 Pa or less, 6 Pa or less, 7 Pa or less, 8 Pa or less, 9 Pa or less, 10 Pa or less, etc.

[0123] T4 is 280°C to 450°C, for example, 280°C, 300°C, 320°C, 340°C, 360°C, 380°C, 400°C, 420°C, 440°C, 450°C, etc.

[0124] v3 does not exceed 5°C / min, for example, not exceeding 0.5°C / min, not exceeding 1°C / min, not exceeding 2°C / min, not exceeding 3°C / min, not exceeding 4°C / min, not exceeding 5°C / min, etc.

[0125] t2 is 50 min to 120 min, for example, it can be 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 110 min, 120 min, etc.

[0126] In some embodiments, during the vacuum sintering stage, the heating rate does not exceed v4, the heating temperature is increased from T4 to T5, and the temperature is kept at t3 time; the heating rate does not exceed v5, and when the sintering temperature reaches T6, the temperature is kept at t4 time; the heating rate does not exceed v6, and when the sintering temperature reaches T7, the temperature is kept at t5 time.

[0127] Furthermore, v4 does not exceed 5°C / min, for example, does not exceed 0.5°C / min, does not exceed 1°C / min, does not exceed 2°C / min, does not exceed 3°C / min, does not exceed 4°C / min, does not exceed 5°C / min, etc.

[0128] T4 is 280°C to 450°C, for example, 280°C, 300°C, 320°C, 340°C, 360°C, 380°C, 400°C, 420°C, 440°C, 450°C, etc.

[0129] T5 is 520°C to 600°C, for example, 520°C, 530°C, 540°C, 550°C, 560°C, 570°C, 580°C, 590°C, 600°C, etc.

[0130] t3 is 10 min to 90 min, for example, it can be 10 min, 20 min, 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, etc.

[0131] v5 does not exceed 4°C / min, for example, does not exceed 0.5°C / min, does not exceed 1°C / min, does not exceed 2°C / min, does not exceed 3°C / min, does not exceed 4°C / min, etc.

[0132] T6 is 900°C to 1150°C, for example, 900°C, 950°C, 100°C, 1050°C, 1100°C, 1150°C, etc.

[0133] t4 is 50 min to 150 min, for example, it can be 50 min, 60 min, 80 min, 90 min, 100 min, 110 min, 120 min, 130 min, 140 min, 150 min, etc.

[0134] v6 does not exceed 4°C / min, for example, does not exceed 0.5°C / min, does not exceed 1°C / min, does not exceed 2°C / min, does not exceed 3°C / min, does not exceed 4°C / min, etc.

[0135] T7 is 1150°C to 1350°C, for example, it may be 1150°C, 1200°C, 1250°C, 1300°C, 1350°C, etc.

[0136] t5 is 30 min to 120 min, for example, it can be 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, 100 min, 110 min, 120 min, etc.

[0137] It can be understood that the pre-solid solution precursor powder obtained by spray granulation is loaded into a graphite boat mold brushed with non-stick boat coating, and then the graphite boat carrying the spheroidized granulated pre-solid solution precursor powder is loaded into a vacuum sintering furnace, and the heating and degreasing stage, vacuum sintering stage and furnace cooling stage are carried out in sequence, and then the metal ceramic block is taken out of the furnace, and the shape of the block is similar to the cavity in the graphite boat.

[0138] It can also be understood that the pre-solid solution precursor powder is sintered in a vacuum sintering furnace. After the vacuum sintering stage is completed, the metal ceramic block will be cooled along with the vacuum sintering furnace to room temperature to obtain a metal ceramic block.

[0139] In said S04:

[0140] It can be understood that the obtained metal ceramic block is placed in the hopper of a double-roll crusher and crushed into powder. The speed adjustment range of the double-roll crusher is 35 rpm to 85 rpm. The crushed powder of the metal ceramic block is placed in a multi-layer ultrasonic oscillation screen to classify the powder. The blocks whose particle size does not meet the screening requirements after classification need to be crushed for the second or third time and then placed in the multi-layer ultrasonic oscillation screen again to classify the powder, and finally the corresponding grade of metal ceramic spray powder is obtained.

[0141] The present application is described in detail below through specific embodiments. The following embodiments are only partial embodiments of the present application and are not limitations of the present application.

[0142] Example 1

[0143] See also Figure 2 The present embodiment provides a metal ceramic spray powder, which includes 77% titanium carbonitride, 10% titanium carbide, and 13% titanium nitride by mass percentage. The titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 1.2 microns. The titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 1 micron. The titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.4 microns.

[0144] In this embodiment, titanium carbonitride is the main phase, and titanium carbide and titanium nitride are the auxiliary phases.

[0145] The preparation method of the metal ceramic spray powder comprises:

[0146] Step 1, weighing titanium carbonitride, titanium carbide and titanium nitride powders as raw material powders according to the above mass percentages, mixing them, adding a dispersant and a molding agent, and mixing them evenly to obtain a prepared raw material, wherein the dispersant is dodecylbenzenesulfonic acid, the molding agent is PEG, the mass fraction of the dispersant in the total amount of the raw material powder is 0.3%, and the mass fraction of the molding agent in the total amount of the raw material powder is 3.5%;

[0147] Step 2, the prepared raw materials are loaded into the ball mill of the ball mill, and a solvent is added and a cemented carbide ball is added for ball milling to obtain a mixed slurry; wherein, the inner shell of the ball mill is made of cemented carbide as a whole; the solvent is ethylene glycol, and the volume mass ratio of the solvent to the total amount of raw material powder is 350ml / Kg; the ball milling is wet milling, using a rolling ball mill, and 87% of the total volume of the solvent is first added during ball milling, and the remaining solvent is added 9h before the end of ball milling; the cemented carbide ball is cemented carbide YG6X, the diameter of the cemented carbide ball is 8.5mm, the ball-to-material ratio is 6:1, the ball milling speed is 75 rpm, and the ball milling time is 52h;

[0148] Step 3, placing the mixed slurry into a spray tower for spray spheroidization granulation to obtain a spherical pre-solid solution precursor powder; the inlet temperature setting range of the sprayer is 230° C., the outlet temperature is set to 115° C., and the centrifugal atomization speed of the spray granulation is 130 Hz, about 7500 rpm;

[0149] Step 4, spray spheroidization and granulation to obtain a spherical pre-solid solution precursor powder is loaded into a graphite boat mold brushed with a non-stick boat coating, and then the graphite boat carrying the spheroidized granulated pre-solid solution precursor powder is loaded into a vacuum sintering furnace, the heating rate and the insulation time are controlled, and the degreasing stage and the vacuum sintering stage are heated in sequence; after the vacuum sintering is completed, the furnace cooling stage is entered, and then the blocks of titanium carbonitride, titanium carbide and titanium nitride-based metal ceramics are taken out of the furnace, and the block shape is similar to the inner cavity of the graphite boat; wherein, the heating and degreasing stage is carried out according to the preheating, vacuuming, heating and insulation processes, preheating to 140°C, the heating rate does not exceed 5°C / min, insulation for 45min, vacuuming to 5 After the pressure is below Pa, the temperature is raised to 360℃, and the heating rate does not exceed 5℃ / min. At 360℃, the temperature is kept for 85min; in the vacuum sintering stage, the heating rate does not exceed 5℃ / min, the heating temperature is raised from 360℃ to 560℃, and the temperature is kept for 50min; the heating rate does not exceed 4℃ / min, and when the sintering temperature reaches 1025℃, the temperature is kept for 100min; the heating rate does not exceed 4℃ / min, and when the sintering temperature reaches 1250℃, the temperature is kept for 75min; after the vacuum sintering stage is completed, the titanium carbonitride, titanium carbide and titanium nitride-based metal ceramic blocks in the furnace will be cooled with the furnace to room temperature to obtain titanium carbonitride, titanium carbide and titanium nitride-based metal ceramic blocks.

[0150] Step 5: crush and sieve the obtained titanium carbonitride, titanium carbide and titanium nitride-based metal ceramic blocks to obtain titanium carbonitride, titanium carbide and titanium nitride-based metal ceramic spray powders.

[0151] Example 2

[0152] See also Figure 3 This embodiment provides a metal ceramic spray powder. According to the mass percentage, the metal ceramic spray powder includes 100% titanium carbonitride, the titanium carbonitride is powder, and the Fsss particle size of the titanium carbonitride powder is 2 microns.

[0153] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0154] Example 3

[0155] The present embodiment provides a metal ceramic spray powder. In terms of mass percentage, the metal ceramic spray powder includes 100% titanium carbide, the titanium carbide is powder, and the Fsss particle size of the titanium carbide powder is 2.5 microns.

[0156] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0157] Example 4

[0158] The present embodiment provides a metal ceramic spray powder. In terms of mass percentage, the metal ceramic spray powder includes 100% titanium nitride, the titanium nitride is powder, and the Fsss particle size of the titanium nitride powder is 1.5 microns.

[0159] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0160] Example 5

[0161] The present embodiment provides a metal ceramic spray powder, which includes 60% titanium carbonitride and 40% titanium carbide by mass percentage; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 0.8 microns; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 1.2 microns.

[0162] In this embodiment, the main phase is titanium carbonitride and the auxiliary phase is titanium carbide.

[0163] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0164] Example 6

[0165] The present embodiment provides a metal ceramic spray powder, which includes 80% titanium carbonitride and 20% titanium nitride by mass percentage; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 3 microns; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 2.8 microns.

[0166] In this embodiment, the main phase is titanium carbonitride and the auxiliary phase is titanium nitride.

[0167] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0168] Example 7

[0169] See also Figure 4 , this embodiment provides a metal ceramic spray powder, which includes 55% titanium carbonitride, 25% titanium carbide, and 20% titanium nitride in terms of mass percentage; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 0.5 microns, the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 0.8 microns, and the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 0.6 microns;

[0170] In this embodiment, titanium carbonitride is the main phase, and titanium carbide and titanium nitride are the auxiliary phases.

[0171] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0172] Example 8

[0173] The present embodiment provides a metal ceramic spray powder, which includes 75% titanium carbonitride, 10% titanium carbide, and 15% titanium nitride by mass percentage; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 3.5 microns, the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 3.8 microns, and the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 2.5 microns;

[0174] In this embodiment, titanium carbonitride is the main phase, and titanium carbide and titanium nitride are the auxiliary phases.

[0175] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0176] Example 9

[0177] The present embodiment provides a metal ceramic spray powder, which includes 95% titanium carbonitride, 2% titanium carbide, and 3% titanium nitride in terms of mass percentage; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 2.2 microns, the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 0.5 microns, and the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 0.2 microns;

[0178] In this embodiment, titanium carbonitride is the main phase, and titanium carbide and titanium nitride are the auxiliary phases.

[0179] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0180] Example 10

[0181] See also Figure 5 The present embodiment provides a metal ceramic spray powder, which includes 51% titanium carbide and 49% titanium carbonitride in terms of mass percentage; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 3.3 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 3.8 microns.

[0182] In this embodiment, the main phase is titanium carbide and the auxiliary phase is titanium carbonitride.

[0183] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0184] Embodiment 11

[0185] The present embodiment provides a metal ceramic spray powder, which includes 98% titanium carbide and 2% titanium nitride by mass percentage; the titanium carbide is a powder with a Fsss particle size of 1.8 microns, and the titanium nitride is a powder with a Fsss particle size of 3.5 microns.

[0186] In this embodiment, the main phase is titanium carbide and the auxiliary phase is titanium nitride.

[0187] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0188] Example 12

[0189] The present embodiment provides a metal ceramic spray powder, which includes 70% titanium carbide, 15% titanium carbonitride, and 15% titanium nitride by mass percentage; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 0.8 microns, the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 1.5 microns, and the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.2 microns;

[0190] In this embodiment, titanium carbide is the main phase, and titanium carbonitride and titanium nitride are the auxiliary phases.

[0191] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0192] Embodiment 13

[0193] The present embodiment provides a metal ceramic spray powder, which includes 52% titanium carbide, 28% titanium carbonitride, and 20% titanium nitride in terms of mass percentage; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 1.2 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 0.8 microns; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.2 microns;

[0194] In this embodiment, titanium carbide is the main phase, and titanium carbonitride and titanium nitride are the auxiliary phases.

[0195] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0196] Embodiment 14

[0197] The present embodiment provides a metal ceramic spray powder, which includes 95% titanium carbide, 4% titanium carbonitride, and 1% titanium nitride by mass percentage; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 3.2 microns, the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 0.8 microns, and the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 0.3 microns;

[0198] In this embodiment, titanium carbide is the main phase, and titanium carbonitride and titanium nitride are the auxiliary phases.

[0199] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0200] Embodiment 15

[0201] The present embodiment provides a metal ceramic spray powder, which includes 90% titanium nitride and 10% titanium carbonitride in terms of mass percentage; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.3 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 3.5 microns.

[0202] In this embodiment, the main phase is titanium nitride and the auxiliary phase is titanium carbonitride.

[0203] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0204] Example 16

[0205] The present embodiment provides a metal ceramic spray powder, which includes 52% titanium nitride and 48% titanium carbide by mass percentage; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.5 microns; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 1.5 microns.

[0206] In this embodiment, the main phase is titanium nitride and the auxiliary phase is titanium carbide.

[0207] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0208] Embodiment 17

[0209] The present embodiment provides a metal ceramic spray powder, which includes 90% titanium nitride, 5% titanium carbonitride, and 5% titanium carbide in terms of mass percentage; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 2 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 1 micron; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 0.6 microns;

[0210] In this embodiment, titanium nitride is the main phase, and titanium carbonitride and titanium carbide are the auxiliary phases.

[0211] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0212] Embodiment 18

[0213] See also Figure 6 The present embodiment provides a metal ceramic spray powder, which includes 52% titanium nitride, 30% titanium carbonitride, and 18% titanium carbide in terms of mass percentage; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.2 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 3 microns; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 2.1 microns;

[0214] In this embodiment, titanium nitride is the main phase, and titanium carbonitride and titanium carbide are the auxiliary phases.

[0215] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0216] Embodiment 19

[0217] The present embodiment provides a metal ceramic spray powder, which includes 75% titanium nitride, 5% titanium carbonitride, and 20% titanium carbide in terms of mass percentage; the titanium nitride is a powder, and the Fsss particle size of the titanium nitride powder is 1.5 microns; the titanium carbonitride is a powder, and the Fsss particle size of the titanium carbonitride powder is 2.2 microns; the titanium carbide is a powder, and the Fsss particle size of the titanium carbide powder is 0.8 microns;

[0218] In this embodiment, titanium nitride is the main phase, and titanium carbonitride and titanium carbide are the auxiliary phases.

[0219] The preparation method of the metal ceramic spray powder is the same as that of Example 1.

[0220] Embodiment 20

[0221] This embodiment is basically the same as Embodiment 1, except that, in this embodiment,

[0222] In step 1, the dispersant is stearic acid, the molding agent is paraffin, the mass fraction of the dispersant to the total amount of the raw material powder is 0.1%, and the mass fraction of the molding agent to the total amount of the raw material powder is 2.5%;

[0223] In step 2, the solvent is hexane, and the volume mass ratio of the solvent to the total amount of raw material powder is 280 ml / kg; the ball milling is wet milling, using a rolling ball mill, 85% of the total volume of the solvent is added during ball milling, and the remaining solvent is added 8 hours before the end of ball milling; the cemented carbide ball is cemented carbide YG6X, the diameter of the cemented carbide ball is 6.25 mm, the ball-to-material ratio is 2.5:1, the ball milling speed is 68 rpm, and the ball milling time is 90 hours;

[0224] In step 3, the inlet temperature of the sprayer is set to 180°C, the outlet temperature is set to 100°C, and the centrifugal atomization speed of the spray granulation is 85 Hz, about 9500 rpm;

[0225] In step 4, the heating and debinding stage is carried out according to the preheating, vacuuming, heating and insulation procedures, preheating to 80°C, heating at a rate not exceeding 10°C / min and insulation for 30 minutes, vacuuming to below 10Pa, heating to 280°C, heating at a rate not exceeding 5°C / min, and insulation at 280°C for 120 minutes; in the vacuum sintering stage, the heating rate does not exceed 5°C / min, the heating temperature is increased from 280°C to 520°C, and insulation is carried out for 90 minutes; the heating rate does not exceed 4°C / min, and when the sintering temperature reaches 900°C, insulation is carried out for 150 minutes; the heating rate does not exceed 4°C / min, and when the sintering temperature reaches 1150°C, insulation is carried out for 120 minutes.

[0226] Embodiment 21

[0227] This embodiment is basically the same as Embodiment 1, except that, in this embodiment,

[0228] In step 1, the dispersant is oleic acid, the molding agent is rubber, the mass fraction of the dispersant to the total amount of raw material powder is 0.5%, and the mass fraction of the molding agent to the total amount of raw material powder is 4.5%;

[0229] In step 2, the solvent is gasoline, and the volume mass ratio of the solvent to the total amount of raw material powder is 500 ml / kg; the ball milling is wet milling, using a rolling ball mill, 90% of the total volume of the solvent is first added during ball milling, and the remaining solvent is added 10 hours before the end of ball milling; the cemented carbide ball is cemented carbide YG6X, the diameter of the cemented carbide ball is 12 mm, the ball-to-material ratio is 10:1, the ball milling speed is 85 rpm, and the ball milling time is 16 hours;

[0230] In step 3, the inlet temperature of the sprayer is set to 280°C, the outlet temperature is set to 130°C, and the centrifugal atomization speed of the spray granulation is 180 Hz, about 5500 rpm;

[0231] In step 4, the heating and debinding stage is carried out according to the preheating, vacuuming, heating and insulation procedures, preheating to 200°C, heating at a rate not exceeding 2°C / min and insulation for 30 minutes, vacuuming to below 3Pa, heating to 450°C, heating at a rate not exceeding 2°C / min, and insulation at 450°C for 50 minutes; in the vacuum sintering stage, the heating rate does not exceed 3°C / min, the heating temperature is increased from 450°C to 600°C, and insulation is carried out for 10 minutes; the heating rate does not exceed 2°C / min, and when the sintering temperature reaches 1150°C, insulation is carried out for 50 minutes; the heating rate does not exceed 2°C / min, and when the sintering temperature reaches 1350°C, insulation is carried out for 30 minutes.

[0232] The above is a detailed introduction to the metal ceramic spray powder and the preparation method thereof provided in the embodiments of the present application. Specific examples are used in this article to illustrate the principles and implementation methods of the present application. The description of the above embodiments is only used to help understand the method of the present application and its core idea; at the same time, for technical personnel in this field, according to the ideas of the present application, there will be changes in the specific implementation methods and application scopes. In summary, the content of this specification should not be understood as a limitation on the present application.

Claims

1. Metal ceramic spray powder, characterized in that: Includes one or more of titanium carbonitride, titanium carbide and titanium nitride.

2. The metal ceramic spray powder according to claim 1, characterized in that: Calculated by mass percentage, the metal ceramic spray powder includes 50% to 100% titanium carbonitride, 0% to 50% titanium carbide, and 0% to 50% titanium nitride; titanium carbonitride is the main phase, and titanium carbide and / or titanium nitride are the auxiliary phases.

3. The metal ceramic spraying powder according to claim 1, characterized in that: Calculated by mass percentage, the metal ceramic spray powder includes 50% to 100% titanium carbide, 0% to 50% titanium carbonitride, and 0% to 50% titanium nitride; titanium carbide is the main phase, and titanium carbonitride and / or titanium nitride are the auxiliary phases.

4. The metal ceramic spraying powder according to claim 1, characterized in that: In terms of mass percentage, the metal ceramic spray powder includes 50% to 100% titanium nitride, 0% to 50% titanium carbonitride, and 0% to 50% titanium carbide; titanium nitride is the main phase, and titanium carbonitride and / or titanium carbide are the auxiliary phases.

5. The metal ceramic spraying powder according to any one of claims 1 to 4, characterized in that: The titanium carbonitride is in the form of a powder, the titanium carbonitride powder having a Fsss particle size of not greater than 4.0 microns; and / or The titanium carbide is in the form of a powder, the titanium carbide powder having a Fsss particle size of not greater than 4.0 microns; and / or The titanium nitride is in the form of powder, and the Fsss particle size of the titanium nitride powder is not greater than 4.0 microns.

6. A method for preparing a metal ceramic spray powder, characterized in that: include: Providing a mixed slurry, the mixed slurry comprising one or more of titanium carbonitride, titanium carbide and titanium nitride; Spray granulate the mixed slurry to obtain pre-solidified precursor powder; The pre-solid solution precursor powder is subjected to a heating and degreasing stage, a vacuum sintering stage and a cooling stage in sequence to obtain a metal ceramic block; The metal ceramic spray powder is obtained by crushing and screening.

7. The method for preparing metal ceramic spray powder according to claim 6, characterized in that: Weigh one or more of titanium carbonitride, titanium carbide and titanium nitride according to the above mass percentage to obtain a raw material powder, add a dispersant and a molding agent to the raw material powder, mix them evenly to obtain a prepared raw material, and wet grind them to obtain a mixed slurry; and / or The mixed slurry is placed in a spray tower for spray spheroidization granulation, the inlet temperature of the spray tower is T1, the outlet temperature is T2, the centrifugal atomization speed of the spray spheroidization granulation is v1, and the frequency is f; and / or The heating and degreasing stage is carried out according to the preheating, vacuuming, heating and insulation procedures, preheating to T3 temperature, the heating rate does not exceed v2, the insulation time is t1, vacuuming to below P, heating to T4, the heating rate does not exceed v3, and at T4 temperature, insulation time t2; and / or During the vacuum sintering stage, the heating rate does not exceed v4, the heating temperature rises from T4 to T5, and is kept warm for t3 time; the heating rate does not exceed v5, when the sintering temperature reaches T6, it is kept warm for t4 time; the heating rate does not exceed v6, when the sintering temperature reaches T7, it is kept warm for t5 time.

8. The method for preparing a metal ceramic spray powder according to claim 7, characterized in that: Add the prepared raw materials into a grinding carbide or stainless steel ball mill of a ball mill, add a solvent and perform ball milling to obtain a mixed slurry; and / or T1 is 180°C to 280°C; and / or T2 is 100°C to 130°C; and / or v1 is 5500 rpm to 9500 rpm; and / or f is between 85 Hz and 180 Hz; and / or T3 is 80°C to 200°C; and / or v2 does not exceed 10℃ / min; and / or t1 is 30 min to 60 min; and / or P is less than 10Pa; and / or T4 is 280°C to 450°C; and / or v3 does not exceed 5℃ / min; and / or t2 is 50 min to 120 min; and / or v4 does not exceed 5℃ / min; and / or T5 is 520°C to 600°C; and / or t3 is 10 min to 90 min; and / or v5 does not exceed 4℃ / min; and / or T6 is 900°C to 1150°C; and / or t4 is 50 min to 150 min; and / or v6 does not exceed 4℃ / min; and / or T7 is 1150°C to 1350°C; and / or t5 is 30min~120min.

9. The method for preparing a metal ceramic spray powder according to claim 8, characterized in that: The dispersant comprises one or more of dodecylbenzenesulfonic acid, stearic acid and oleic acid; and / or The molding agent is one or more of rubber, paraffin and PEG; and / or The solvent includes one or more of gasoline, ethylene glycol and hexane.

10. The method for preparing a metal ceramic spray powder according to claim 9, characterized in that: In the mixed slurry, the ratio of solid to liquid is (5-7):(5-3); and / or The mass fraction of the dispersant in the total amount of the raw material powder is 0.1% to 0.5%; and / or The mass fraction of the molding agent to the total amount of raw material powder is 2.5% to 4.5%; and / or The volume mass ratio of the solvent to the total amount of the raw material powder is 280ml / Kg to 500ml / Kg; and / or During ball milling, 85% to 90% of the total volume of the solvent is first added, and the remaining solvent is added 8 to 10 hours before the end of ball milling; and / or The ball mill is a rolling ball mill or a vertical stirring ball mill, the diameter of the carbide balls is 6.25 mm to 12 mm, the ball-to-material ratio is 2.5:1 to 10:1, the ball milling speed is 68 to 85 rpm, and the ball milling time is 16 h to 90 h.

Images