CN115838888A - TiC-based thermal spraying powder and preparation method thereof - Google Patents
TiC-based thermal spraying powder and preparation method thereof Download PDFInfo
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Abstract
The invention discloses TiC-based thermal spraying powder and a preparation method thereof, wherein the thermal spraying powder comprises the following components in mass: 55-75% of TiC, 25-45% of FeCrAlNi and the following elements in mass percent: 44-60% of Ti, 11-15% of C, 18-30% of Fe, 4-8% of Cr, 2-4% of Ni and 1-2% of Al. The preparation method comprises the following steps: preparing raw materials, and putting the weighed raw materials into a three-dimensional mixer for dry mixing uniformly to obtain mixed powder; filling the mixed powder into a self-propagating high-temperature synthesis device, vacuumizing the device, filling argon to form a protective atmosphere, preheating the mixed powder to 500-700 ℃, electrifying a tungsten wire to strike a fire, triggering a self-propagating high-temperature synthesis reaction, and controlling the reaction process by using an external electric field in the reaction process to obtain ceramic powder; and (4) screening the ceramic powder to obtain the thermal spraying powder with the particle size of 15-45 mu m. Solves the problems of poor compactness, poor powder appearance and uneven components of the TiC-based thermal spraying powder prepared by the prior art.
Description
Technical Field
The invention relates to the technical field of surface engineering, in particular to TiC-based thermal spraying powder and a preparation method thereof.
Background
In the wear-resistant and corrosion-resistant surface strengthening industry, the commonly applied coating material is a carbide-based cermet material which is made of WC and Cr 3 C 2 And metal carbides such as VC, tiC and the like are used as hard phases to improve the strength of the coating, and metal or metal powder such as Co, cr, ni, fe and the like is used as a binder phase to improve the corrosion resistance or other properties of the coating. The metal ceramic powder for thermal spraying is required to have certain mechanical strength and higher apparent density so as to ensure the compactness and strength of a coating, and then the particle distribution, the components and the morphology are adjusted according to different use working conditions.
In metal carbide, tiC has quite excellent wear resistance and hardness, and has been widely applied to hard alloy materials due to high melting point and good chemical stability, but in the field of surface strengthening, the produced thermal spraying powder has the problems of poor compactness and poor powder morphology due to poor wettability with most metals.
The thermal spraying powder has more production and preparation processes, and the properties of the thermal spraying powder produced and prepared have larger differences with the difference of the manufacturing processes. At present, the common process routes for preparing the metal ceramic thermal spraying powder comprise agglomeration sintering, sintering crushing, melting crushing and the like.
In a conventional production process route, an agglomeration sintering process adopts a spray drying granulation mode, the prepared powder has high sphericity, different component raw materials in the powder are combined through a forming agent, and the applicability is larger, but the agglomeration sintering process route is mostly to sinter a hard phase and a bonding phase after directly and mechanically mixing the hard phase and the bonding phase, for example, in Chinese patent with publication number CN111826571B and name of titanium carbide-iron chromium aluminum thermal spraying powder and a preparation method thereof, centrifugal spray granulation and vacuum furnace sintering are used, but the problem of poor wettability between the bonding phase and the hard phase is not solved, the prepared TiC-based thermal spraying powder often has the problems of insufficient mechanical strength and poor compactness, the problems of poor spraying efficiency, low coating hardness or large brittleness and the like are further caused, and the TiC-based thermal spraying powder is difficult to be applied to actual working conditions and replaces tungsten-based powder; meanwhile, because the loose packing density of the TiC-based powder is low, a special large-capacity tool is used under the preparation condition of an agglomeration sintering method, or the production efficiency is low, so that the large-batch production and supply are difficult to realize.
The two process routes of sintering and crushing and melting and crushing are suitable for producing high-density powder materials, but the powder prepared by the method is irregular in shape, poor in sphericity and fluidity, not beneficial to thermal spraying, and difficult to be used in batch production and supply, and spheroidization treatment in flame or plasma arc is needed, so that the manufacturing cost is greatly increased, and batch production and supply are difficult to realize. In conclusion, the TiC-based thermal spraying powder manufactured by the conventional method has a plurality of manufacturing and product performance problems.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a preparation method of TiC-based thermal spraying powder, which aims to solve the problems of poor compactness, poor powder morphology and non-uniform components of the TiC-based thermal spraying powder prepared by the prior art.
In order to achieve the purpose, the invention adopts the specific scheme that:
a TiC-based thermal spray powder comprising, by mass: 55-75% of TiC, 25-45% of FeCrAlNi and the following elements in mass percent: 44-60% of Ti, 11-15% of C, 18-30% of Fe, 4-8% of Cr, 2-4% of Ni and 1-2% of Al.
A preparation method of TiC-based thermal spraying powder mainly comprises the following steps:
(1) Preparing raw materials: titanium powder, which accounts for 44% -60% of the total weight of the composite powder; carbon powder, which accounts for 11 to 15 percent of the total weight of the composite powder; iron powder, which accounts for 18-30% of the total weight of the composite powder; chromium powder accounting for 4-8% of the total weight of the composite powder; nickel powder, which accounts for 2-4% of the total weight of the composite powder; aluminum powder accounting for 1-2% of the total weight of the composite powder; putting the weighed raw materials into a three-dimensional mixer, and uniformly mixing the raw materials in a dry mode to obtain mixed powder;
(2) Putting the mixed powder into a self-propagating high-temperature synthesis device, vacuumizing the device, filling argon to form a protective atmosphere, preheating the mixed powder to 500-700 ℃, electrifying and igniting a tungsten filament to trigger a self-propagating high-temperature synthesis reaction, and controlling the reaction process by using an external electric field in the reaction process to obtain ceramic powder;
(3) And sieving the ceramic powder to obtain the thermal spraying powder of 15-45 microns.
Preferably, in the step (1), the average size of the titanium powder is 100 to 130 μm, the average size of the carbon powder is 30 to 50 μm, the average size of the iron powder is 50 to 80 μm, the average size of the chromium powder is 40 to 70 μm, the average size of the nickel powder is 50 to 80 μm, and the average size of the aluminum powder is 60 to 90 μm.
Preferably, in the step (1), the three-dimensional mixer is a double-helix conical mixer, and the raw materials are dry-mixed by adopting an asymmetric double-helix stirring structure.
Preferably, in the step (2), the voltage of the applied electric field is 300 to 500KV.
Preferably, in the step (2), the device is vacuumized until the absolute pressure is less than 30Pa, and then argon is injected until micro negative pressure is formed to form protective atmosphere.
Preferably, in the step (2), the self-propagating high-temperature synthesis reaction time is 280-340s, the temperature rapidly rises to 1280-1320 ℃ within 20-50s, the temperature starts to be reduced within 50-120s, the temperature stably reacts within the temperature range of 1110-1150 ℃ within 100-280s, the temperature starts to be reduced after 280-340 s, and the ceramic powder is obtained after the ceramic powder is naturally cooled to the room temperature.
Has the beneficial effects that:
(1) The preparation method can be used for preparing the thermal spraying powder simply, conveniently, efficiently and at low cost;
(2) According to the invention, the size and proportion of the raw material simple substance powder, the cooling rate after reaction and the applied electric field voltage are controlled, so that the reduction of tiny particles in the appearance of the finished product powder can be realized, and the control of phase composition distribution can be realized by controlling the reaction rate; through the screening treatment after the reaction, the control on the powder particle size distribution can be realized, and compared with the traditional manufacturing mode, the control on the powder performance is more visual and convenient;
(3) According to the invention, the simple substance powders are uniformly mixed by three-dimensional mixing and double-helix stirring, and the prepared thermal spraying powder has good component uniformity; because of combustion reaction in the self-propagating high-temperature synthesis, the powder has higher density, relatively round single-particle appearance and good fluidity; because the powder prepared by the self-propagating high-temperature synthesis method has strong chemical bonds on a metal/ceramic interface, the bonding property of TiC and a metal phase is better, and the problem of poor wear resistance of a coating layer caused by poor interface bonding between titanium carbide and a binding phase and weak intergranular fracture resistance of the coating layer prepared by the traditional production mode is solved;
(4) The self-propagating high-temperature synthesis method can realize the mass continuous production of the thermal spraying powder.
Drawings
Fig. 1 is a microstructure diagram of the thermal spray powder prepared in example 1.
FIG. 2 is a microstructure diagram of a coating prepared using the thermal spray powder prepared in example 1 and using plain carbon steel as a substrate.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to specific embodiments, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, belong to the scope of the present invention.
A TiC-based thermal spraying powder applied to an erosion-resistant coating of a water-cooled wall of a boiler and a preparation method thereof belong to the technical field of surface engineering, the preparation method of the powder adopts a self-propagating high-temperature synthesis technology, and the preparation method of the component powder (with the specification of 15-45 microns) can improve the wear resistance of a metal ceramic coating prepared by supersonic flame spraying by 50 percent, thereby obtaining important application in the fields of surface wear resistance and erosion-resistant protection.
The invention provides TiC-based thermal spraying powder which comprises the following components in mass: tiC accounts for 55-75%, and FeCrAlNi accounts for 25-45%. The content of each element by mass is as follows: 44-60% of Ti, 11-15% of C, 18-30% of Fe, 4-8% of Cr, 2-4% of Ni and 1-2% of Al.
The optimal mixture ratio of each component by mass is as follows: tiC accounts for 64%, fe accounts for 25%, cr accounts for 7%, ni accounts for 3%, and Al accounts for 1%.
The invention also provides a preparation method of the TiC-based thermal spraying powder, which comprises the following steps:
(1) Preparing raw materials: titanium powder, which accounts for 44-60% of the total weight of the composite powder; carbon powder which accounts for 11 to 15 percent of the total weight; iron powder, which accounts for 18-30% of the total weight; chromium powder accounting for 4-8% of the total weight; nickel powder, which accounts for 2-4% of the total weight; aluminum powder accounts for 1-2% of the total weight.
(2) The raw material simple substance powder is placed in a three-dimensional mixer for dry mixing, so that the raw material powder is uniformly mixed to obtain mixed powder, in detail, the used three-dimensional mixer is a double-spiral conical mixer, an asymmetric double-spiral stirring structure is adopted, components with large specific gravity differences in the raw material simple substance powder are uniformly mixed more properly, and the mixing time is 4 hours.
(3) Putting the mixed powder prepared in the step (2) into a tubular graphite container lined with ceramic paper, and placing the graphite container into a self-propagating high-temperature synthesis device;
vacuumizing the device and filling argon to form a protective atmosphere, minimizing the probability of oxidation reaction, reducing the generation of impurities, preheating the powder to 700 ℃, electrifying and igniting a tungsten wire to trigger the self-propagating high-temperature synthesis reaction to start, controlling the reaction progress by using an external electric field in the reaction process, and preparing the thermal spraying powder after the reaction is finished.
The particle size of raw material simple substance titanium powder, carbon powder and aluminum powder and the voltage of an external electric field can be controlled to further control the speed and the product of the self-propagating high-temperature synthesis reaction.
(4) And (4) screening the powder prepared in the step (3) to obtain a finished product.
Example 1
A preparation method of TiC-based thermal spraying powder comprises the following steps:
(1) Weighing 51.2 percent of Ti powder (with the average size of 110 mu m), 12.8 percent of carbon powder (with the average size of 40 mu m), 25 percent of Fe powder (with the average size of 60 mu m), 7 percent of Cr powder (with the average size of 50 mu m), 3 percent of Ni powder (with the average size of 60 mu m) and 1 percent of Al powder (with the average size of 70 mu m) by weight;
(2) Mixing the powder for 4 hours by using a double-helix conical mixer to prepare mixed powder;
(3) Laying ceramic paper on the inner part of a tubular graphite boat, putting the mixed powder into the boat, connecting a tungsten wire into the powder, externally connecting the tungsten wire with the power, and putting the boat filled with the powder into a self-propagating high-temperature synthesis device;
the device is firstly vacuumized (the absolute pressure is less than 30 Pa), then argon is filled until micro negative pressure (relative pressure is-5 to-15 KPa) is formed to form protective atmosphere, and the damage of equipment caused by the thermal expansion of gas after the reaction is started is avoided;
electrifying a tungsten wire to ignite, triggering a reaction to start, spreading combustion waves in the powder from an ignition part, counting for 300s from the beginning of the reaction to the end of the reaction, wherein the highest temperature of materials is about 1300 ℃ during the reaction, the temperature is sharply increased to the highest temperature during 20-50s, the temperature is reduced at 50-100s, an external electric field is started at 100s, the voltage is 300KV, the reaction is stably performed at 1120-1130 ℃ during 100-300s, the temperature is gradually reduced after 300s, and the powder is taken out after naturally cooling to below 40 ℃;
(4) And sieving the synthetic powder to 15-45 μm to obtain titanium carbide-based thermal spraying powder product.
The prepared thermal spray powder was subjected to composition analysis, and the main components and proportions thereof are shown in table 1 below.
TABLE 1 ingredient Table of thermal spray powder prepared in this example
XRD analysis is carried out on the prepared thermal spraying powder, and the main phases of the powder comprise TiC, fe (Cr) and Fe 3 C. FeTi, al (Fe), al (Ni), etc.
The HVOF equipment is used for preparing the coating, spraying parameters are optimized, the common carbon steel is used as a substrate to prepare the coating, the microhardness Hv0.3 1043-1301 of the coating is high, and the wear coefficient is 0.89.
Example 2
A preparation method of TiC-based thermal spraying powder comprises the following steps:
(1) Weighing 51.2% of Ti powder (with an average size of 120 mu m), 12.8% of carbon powder (with an average size of 50 mu m), 25% of Fe powder (with an average size of 70 mu m), 7% of Cr powder (with an average size of 40 mu m), 3% of Ni powder (with an average size of 50 mu m) and 1% of Al powder (with an average size of 60 mu m) by weight;
(2) Mixing the powder for 4 hours by using a double-helix conical mixer to prepare mixed powder;
(3) Laying ceramic paper on the inner part of a tubular graphite boat, putting the mixed powder into the boat, connecting a tungsten wire into the powder, externally connecting the tungsten wire with the power, and putting the boat filled with the powder into a self-propagating high-temperature synthesis device;
the device is firstly vacuumized (the absolute pressure is less than 30 Pa), then argon is filled until micro negative pressure (relative pressure is-5 to-15 KPa) is formed to form protective atmosphere, and the damage of equipment caused by the thermal expansion of gas after the reaction is started is avoided;
electrifying a tungsten wire to ignite, triggering a reaction to start, starting spreading of combustion waves in the powder from an ignition part, totaling 240s from the beginning of the reaction to the end of the reaction, enabling the highest temperature of materials to be about 1300 ℃ during the reaction, rapidly increasing the temperature to the highest temperature within 20-50s, starting cooling within 50-100s, starting an external electric field within 100s, enabling the materials to stably react within 1120-1130 ℃ during 100-240s at a voltage of 400KV, starting gradually cooling after 240s, naturally cooling to below 40 ℃, and taking out the powder;
(4) Sieving the synthetic powder to obtain the titanium carbide-based thermal spraying powder finished product with the specification of 15-45 mu m.
The prepared thermal spray powder was subjected to composition analysis, and the main components and proportions thereof are shown in table 2 below.
TABLE 2 ingredient Table of thermal spray powder prepared in this example
| Composition (A) | Ti | C | Fe | Cr | Ni | Al |
| Ratio/%) | Balance | 11.8 | 23.4 | 7.2 | 2.7 | 0.9 |
XRD analysis is carried out on the powder, and the main phases of the powder comprise TiC, fe (Cr) and Fe 3 C. FeTi, al (Fe), al (Ni), etc.
And preparing a coating by using HVOF equipment, optimizing spraying parameters, and preparing the coating by using common carbon steel as a substrate, wherein the microhardness Hv0.3-1325 of the coating and the wear coefficient are 0.80.
Example 3
A preparation method of TiC-based thermal spraying powder comprises the following steps:
(1) Weighing 55 percent of Ti powder (with the average size of 110 mu m), 9 percent of carbon powder (with the average size of 40 mu m), 25 percent of Fe powder (with the average size of 60 mu m), 7 percent of Cr powder (with the average size of 50 mu m), 3 percent of Ni powder (with the average size of 60 mu m) and 1 percent of Al powder (with the average size of 70 mu m) by weight;
(2) Mixing the powder for 4 hours by using a double-helix conical mixer to prepare uniformly mixed powder;
(3) Laying ceramic paper on the inner part of a tubular graphite boat, putting the mixed powder into the boat, connecting a tungsten wire into the powder, externally connecting the tungsten wire with the power, and putting the boat filled with the powder into a self-propagating high-temperature synthesis device;
the device is firstly vacuumized (the absolute pressure is less than 30 Pa), then argon is filled until micro negative pressure (relative pressure is-5 to-15 KPa) is formed to form protective atmosphere, and the damage of equipment caused by the thermal expansion of gas after the reaction is started is avoided;
electrifying a tungsten wire to ignite, triggering a reaction to start, spreading combustion waves in the powder from an ignition part, counting 280s from the beginning of the reaction to the end of the reaction, wherein the highest temperature of materials in the reaction is about 1320 ℃, the temperature is sharply increased to the highest temperature in the period of 20-50s, the temperature is reduced at 50-100s, an external electric field is started in the period of 100s, the voltage is 500KV, the reaction is stably performed in the range of 1130-1150 ℃ in the period of 100-280s, the temperature is gradually reduced after 280s, and the powder is taken out after being naturally cooled to below 40 ℃;
(4) And screening the synthetic powder to obtain the titanium carbide-based thermal spraying powder finished product with the specification of 15-45 mu m.
The prepared thermal spray powder was subjected to composition analysis, and the main components and proportions thereof are shown in table 3 below.
TABLE 3 ingredient Table of thermal spray powder prepared in this example
| Composition (I) | Ti | C | Fe | Cr | Ni | Al |
| Ratio/%) | Balance | 8.9 | 23.6 | 7.1 | 3.2 | 1.1 |
XRD analysis is carried out on the powder, and the main phase of the powder comprises Ti 2 C、Fe(Cr)、Fe 3 C. FeTi, al (Fe), al (Ni), etc.
Using HVOF equipment to prepare a coating, optimizing spraying parameters, and using common carbon steel as a substrate to prepare the coating, wherein the microhardness Hv0.3-1282 and the wear coefficient are 0.99.
Example 4
A preparation method of TiC-based thermal spraying powder comprises the following steps:
(1) Weighing 48 percent of Ti powder (with the average size of 110 mu m), 16 percent of carbon powder (with the average size of 40 mu m), 25 percent of Fe powder (with the average size of 60 mu m), 7 percent of Cr powder (with the average size of 50 mu m), 3 percent of Ni powder (with the average size of 60 mu m) and 1 percent of Al powder (with the average size of 70 mu m) by weight;
(2) Mixing the powder for 4 hours by using a double-helix conical mixer to prepare uniformly mixed powder;
(3) Laying ceramic paper on the inner part of a tubular graphite boat, putting the mixed powder into the boat, connecting a tungsten wire into the powder, externally connecting the tungsten wire with the power, and putting the boat filled with the powder into a self-propagating high-temperature synthesis device;
the device is firstly vacuumized (the absolute pressure is less than 30 Pa), then argon is filled until micro negative pressure (relative pressure is-5 to-15 KPa) is formed to form protective atmosphere, and the damage of equipment caused by the thermal expansion of gas after the reaction is started is avoided;
electrifying a tungsten wire to ignite, triggering a reaction to start, starting spreading of combustion waves in the powder from an ignition part, counting for 340s from the beginning of the reaction to the end of the reaction, enabling the highest temperature of materials to be about 1290 ℃, rapidly increasing the temperature to the highest temperature during 20-50s, starting cooling within 50-120s, starting an external electric field at 120s, enabling the materials to stably react within 1110-1130 ℃ during 300KV and 120-340s, starting gradual cooling after 340s, naturally cooling to below 40 ℃, and taking out the powder;
(4) Sieving the synthetic powder to obtain a titanium carbide-based thermal spraying powder finished product with the specification of 15-45 mu m;
the prepared thermal spray powder was subjected to composition analysis, and the main components and proportions thereof are shown in table 4 below.
Table 4 composition table of thermal spray powder prepared in this example
| Composition (I) | Ti | C | Fe | Cr | Ni | Al |
| Ratio/%) | Balance | 14.8 | 22.9 | 6.8 | 3.1 | 1.0 |
XRD analysis of the powder was carried out, the major phase of the powder comprising TiC 2 、Fe(Cr)、Fe 3 C. FeTi, al (Fe), al (Ni), etc.;
the HVOF equipment is used for preparing the coating, spraying parameters are optimized, the common carbon steel is used as a substrate to prepare the coating, the microhardness Hv0.3-1150 of the coating is obtained, and the wear coefficient is 1.07.
The foregoing is merely a preferred embodiment of the invention and is not to be construed as limiting the invention in any way. All equivalent changes or modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A TiC-based thermal spray powder is characterized in that the powder components by mass: 55-75% of TiC, 25-45% of FeCrAlNi and the following elements in mass percent: 44-60% of Ti, 11-15% of C, 18-30% of Fe, 4-8% of Cr, 2-4% of Ni and 1-2% of Al.
2. A preparation method of TiC-based thermal spraying powder is characterized by mainly comprising the following steps:
(1) Preparing raw materials: titanium powder, which accounts for 44-60% of the total weight of the composite powder; carbon powder, which accounts for 11 to 15 percent of the total weight of the composite powder; iron powder accounting for 18 to 30 percent of the total weight of the composite powder; chromium powder accounting for 4 to 8 percent of the total weight of the composite powder; nickel powder accounting for 2 to 4 percent of the total weight of the composite powder; aluminum powder accounting for 1 to 2 percent of the total weight of the composite powder; putting the weighed raw materials into a three-dimensional mixer, and uniformly mixing the raw materials to obtain mixed powder;
(2) The method comprises the following steps of putting mixed powder into a self-propagating high-temperature synthesis device, vacuumizing the device, filling argon into the device to form a protective atmosphere, preheating the mixed powder to 500-700 ℃, electrifying a tungsten wire to strike fire, triggering a self-propagating high-temperature synthesis reaction, and controlling the reaction process by using an external electric field in the reaction process to obtain ceramic powder;
(3) And screening the ceramic powder to obtain the thermal spraying powder with the particle size of 15-45 mu m.
3. A TiC-based thermal spray powder preparation method according to claim 2, characterized in that in step (1), the average size of titanium powder is 100 to 130 μm, the average size of carbon powder is 30 to 50 μm, the average size of iron powder is 50 to 80 μm, the average size of chromium powder is 40 to 70 μm, the average size of nickel powder is 50 to 80 μm, and the average size of aluminum powder is 60 to 90 μm.
4. A TiC-based thermal spray powder preparation method according to claim 2, characterized in that, in step (1), the selected three-dimensional mixer is a double helix conical mixer, and an asymmetric double helix stirring structure is adopted to dry mix the raw materials.
5. A TiC-based thermal spray powder preparation method according to claim 2, characterized in that in step (2), the applied electric field voltage is 300 to 500KV.
6. A TiC-based thermal spray powder preparation method as claimed in claim 2, wherein in step (2), the device is evacuated to an absolute pressure of less than 30Pa, and then argon gas is injected to a slight negative pressure to form a protective atmosphere.
7. A TiC-based thermal spraying powder preparation method as claimed in claim 2, wherein in step (2), the self-propagating high temperature synthesis reaction time is 280 to 340s, the temperature in 20 to 50s rapidly rises to 1280 to 1320 ℃, the temperature starts to decrease in 50 to 120s, the reaction is stabilized in 100 to 280s in a temperature range of 1110 to 1150 ℃, the temperature starts to decrease after 280 to 340s, and the ceramic powder is obtained after natural cooling to room temperature.
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Application publication date: 20230324 |