CN108213410B - Based on (Ti, Me) CN-MxC-Co coating spraying and 3D printing cermet material and preparation method thereof - Google Patents
Based on (Ti, Me) CN-MxC-Co coating spraying and 3D printing cermet material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a (Ti, Me) -based CN-MxThe coating spraying and 3D printing metal ceramic material of C-Co and the preparation method thereof are provided, the metal ceramic material is spherical powder, and the components by mass percent comprise: (Ti, Me) CN-MxC-Co and at least one selected from Ni, Mo and Fe, the content of (Ti, Me) CN is 20-94%, MxThe content of C is 1-40%, and the content of Co and at least one of Ni, Mo and Fe is 5-40%; the metal Me is at least one of W, Mo, Ta, V, Cr, Nb and Zr; the carbide MxC is at least one of WC, MoC, Mo2C, TaC, Cr3C2, NbC, VC and ZrC. The material is prepared by mixing, drying, spheroidizing powder and sintering. The spheroidization of the powder can be carried out by adopting methods such as roller spheroidization, radio frequency plasma spheroidization or spray granulation spheroidization. The cermet material provided by the invention is used as a coating material, improves the binding force between the coating and the substrate, is used as a 3D printing material, and can improve the quality of a 3D printing product.
Description
Technical Field
The invention belongs to the field of thermal spraying coating materials and 3D printing materials, and particularly relates to a metal ceramic composite alloy material for coating spraying and 3D printing and a preparation method thereof.
Background
Failure modes of metal workpieces are mainly caused by wear. Although the wear resistance can be improved by means of heat treatment, modification treatment, doping and the like, the improvement of the surface hardness is very limited, and the potential exertion is limited. Furthermore, the coating technique of the surface of the workpiece is developed, and the cermet is also used as a commonly used coating material. Generally, the higher the hardness of the cermet material is, the stronger the deformation resistance of the surface of the cermet material is, and the better the wear resistance is, and when the cermet material is used as a coating, the better the wear resistance of the surface of a workpiece is improved; the higher the toughness (strength and toughness), the better the impact resistance. Therefore, hardness and toughness have become important indicators for evaluating the performance of cermets. The traditional metal ceramic coating material is directly used after being simply mixed due to the main raw material powder with the conventional size and shape. Its advantages are low cost, and high adhesion between sprayed material and substrate, and complex reaction during thermal spraying. These problems will lead to the deterioration of the coating performance, and thus the cracking and falling off of the coating material during the use of the workpiece will occur, which will affect the use of the product.
For 3D printing of cermet materials, it is essentially a rapid prototyping technique. The traditional powder metallurgy technology is difficult to realize integrated preparation and forming for some metal ceramic workpieces with complex shapes, and the adopted traditional powder metallurgy raw materials are difficult to meet the requirements of the 3D printing technology on the raw materials. In the 3D printing rapid forming process, the raw materials of the traditional powder metallurgy hardly reach the high compactness and the high mechanical property of the traditional powder metallurgy product. Therefore, uniform spherical powder is generally required as a metal ceramic raw material for 3D printing, and the conventional powder spheroidizing method (such as airflow spheroidizing) is high in cost and has great limitation on commercial application.
Disclosure of Invention
The invention aims to provide a (Ti, Me) CN-M-based material aiming at the current situation and the defects of the prior artxThe coating spraying and 3D printing cermet material of C-Co and the preparation method thereof are used for improving the performance of the coating and the binding force between the coating and a substrate, meeting the requirements of 3D printing on the cermet raw materials, improving the quality of 3D printing products and reducing the cost of the raw materials.
The invention provides (Ti, Me) -based CN-MxThe C-Co coating spraying and 3D printing cermet material is spherical powder and comprises the following components in percentage by mass: (Ti, Me) CN-MxC-Co and at least one selected from Ni, Mo and Fe, the content of (Ti, Me) CN is 20-94%, MxThe content of C is 1-40%, and the content of Co and at least one of Ni, Mo and Fe is 5-40%; the metal Me is at least one of W, Mo, Ta, V, Cr, Nb and Zr; the carbide MxC in the TiCN-MxC-Co is at least one of WC, MoC, Mo2C, TaC, Cr3C2, NbC, VC and ZrC.
In the technical scheme of the metal ceramic composite alloy spherical powder, the content of Me in the (Ti, Me) CN is preferably controlled within the range of 5-40% of the total mass of Ti and Me.
The preparation method of the cermet material comprises the following process steps:
(1) mixing and drying, namely adding the raw material powder and a ball milling agent in a formula amount into ball milling mixing equipment, fully ball milling and mixing to obtain a mixture, and fully drying the obtained mixture in drying equipment to obtain a dried mixture;
(2) spheroidizing powder, namely crushing the dried mixture obtained in the step (1), sieving the crushed mixture by using a 300-600-mesh sieve, feeding the sieved powder material into roller spheroidizing equipment to spheroidize the powder, and sieving the powder to remove spherical powder with the particle size of more than 30 meshes and less than 120 meshes, thereby obtaining spherical powder with uniform particle size distribution;
and adding a forming agent before granulation;
(3) sintering, namely putting the spherical powder prepared in the step (2) into a vacuum sintering furnace, vacuumizing to below 1 x 10 < -1 > Pa or continuously introducing Ar gas to keep the air pressure in the vacuum sintering furnace at 500-1200 Pa, heating to 350-600 ℃, keeping the temperature for 2-8 hours to remove the added forming agent, heating to 800-1300 ℃ to fire for 0.5-4 hours under the vacuum of below 1 x 10 < -1 > Pa, and cooling along with the furnace to obtain the spherical powder of the metal ceramic composite alloy;
or comprises the following process steps:
(1) mixing and drying, namely adding the raw material powder and the ball milling agent in a formula amount into ball milling mixing equipment, fully ball milling and mixing to obtain a mixture, and fully drying the obtained mixture in drying equipment to obtain a dried mixture;
(2) pressing and forming, namely sieving the mixture prepared in the step (1) by using a 30-80-mesh sieve for granulation, and then pressing and forming the sieved granules;
and adding a forming agent before granulation;
(3) firing and crushing, namely placing the formed blank obtained in the step (2) into a vacuum sintering furnace, vacuumizing to below 1 x 10 < -1 > Pa or continuously introducing Ar gas to keep the air pressure in the vacuum sintering furnace at 500-1200 Pa, heating to 350-600 ℃, keeping the temperature for 2-8 hours to remove a forming agent, then heating to 800-1300 ℃ to fire for 0.5-4 hours under the vacuum of below 1 x 10 < -1 > Pa, then cooling along with the furnace, and crushing the sintered formed blank into a particle material of 30-100 micrometers;
(4) performing radio frequency plasma spheroidization, namely placing the granular material with the grain size of 30-100 microns obtained in the step (3) in a radio frequency plasma spheroidizing device for spheroidization under the protection of argon to obtain spherical powder of the metal ceramic composite alloy;
or comprises the following process steps:
(1) mixing and drying, namely adding the raw material powder, the ball grinding agent and the forming agent in the formula ratio into ball-milling mixing equipment, and fully ball-milling and mixing to obtain mixed slurry;
(2) spray granulation, namely feeding the slurry obtained in the step (1) into a centrifugal spray granulation dryer for spray granulation to obtain spherical powder;
(3) and (3) sintering heat treatment, namely placing the spherical powder obtained in the step (2) in a vacuum sintering furnace, heating to 800-1300 ℃ at the heating rate of 3-10 ℃/min, sintering for 0.5-5 h, and then cooling to room temperature along with the furnace to obtain the spherical powder of the metal ceramic composite alloy.
In the technical scheme of the preparation method of the metal ceramic composite alloy spherical powder, the ball-milling agent added in the process of preparing the mixture by ball-milling and mixing is preferably alcohol or acetone; the forming agent added in the mixing process or the forming process is preferably one of polyethylene glycol, paraffin, buna rubber and SD (secure digital) rubber, and the adding amount of the forming agent is preferably controlled within the range of 0.5-5% of the total mass of the raw material powder.
In the preparation method of the metal ceramic composite alloy spherical powder, a spherical roller is adopted for powder sphericizing, a roller device with a roller wall of a jacket structure is preferably adopted, in the process of sphericizing, circulating water flow with the temperature of 50-80 ℃ is introduced into the jacket, the rotating speed of the roller is 15-45 r/min, and the time for sphericizing is 10-20 min.
In the preparation method of the metal ceramic composite alloy spherical powder, the operation priority control of the radio frequency plasma spheroidizing device is as follows: the power is 30-100 KW, the argon working flow is 15-40 slpm, the argon protection flow is 100-200 slpm, the negative pressure of the system is 0.1-0.5 atm, the powder feeding gas flow is 2-8 slpm, and the powder feeding speed is 20-60 g/min; the temperature of the discharge plasma of the radio frequency plasma spheroidizing device is preferably controlled to be not lower than 3200 ℃.
In the preparation method of the metal ceramic composite alloy spherical powder, the operation priority control of the centrifugal spray granulation dryer is as follows: the inlet temperature is 100-350 ℃, the outlet temperature is 80-250 ℃, the rotating speed is 10-25 kr/min, and the slurry feeding speed is 5-22 ml/min.
Compared with the prior art, the invention has the following beneficial effects:
1. the components of the spherical powder of the metal ceramic composite alloy prepared by the method can be adjusted according to needs, and meanwhile, because the sintering after the spheroidization belongs to solid phase diffusion sintering, the components are less segregated and have high uniformity, so that the microstructure of the product after spraying or 3D printing is more uniform, and the product performance consistency is higher.
2. As a 3D printing material, the metal ceramic composite alloy spherical powder provided by the invention overcomes the defects of high porosity and poor mechanical property of a carbonitride material under the condition of 3D printing rapid forming.
3. The metal ceramic composite alloy spherical powder provided by the invention is solid solution powder, so that the bonding property of the coating and the matrix can be improved, the stress between the coating and the matrix is effectively reduced, and the performance of the coating is improved. Simultaneously can adjust the mechanical properties of the coating such as toughness and the like
4. The preparation method of the metal ceramic composite alloy spherical powder provided by the invention has the advantages of simple process, low requirement on equipment and greatly reduced preparation cost of the spherical powder, and is particularly suitable for industrial production.
Drawings
FIG. 1 shows the spherical powder obtained in example 2
Detailed Description
The following examples further illustrate the cermet composite alloy spherical powder and the preparation method thereof according to the present invention.
In the following examples, the percentages of the components in the chemical formula of the cermet-containing composite alloy before the components represent the mass percentages of the components in the nitrogen-containing master alloy, and the percentages not written before the components represent the rest.
Example 1
Proportioning, mixing and drying
Weighing 4kg of Co powder and 6kg of Ti (C)0.7,N0.3) Adding 500g of polyethylene glycol into the powder, uniformly mixing the raw materials by a ball milling and mixing method, milling the mixture with alcohol, and then drying the mixture in vacuum to obtain a mixture;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 300; then, the powder is spheroidized by adopting a roller spheroidizing method, and is sieved by a 30-mesh sieve, and the powder passing through the sieve is taken; sieving with a 50-mesh sieve, and taking the powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the step II into a vacuum sintering furnace, vacuumizing to below 1 x 10 < -1 > Pa, heating to 600 ℃, and keeping the temperature for 2 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 800 ℃ for firing for 4 hours; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process adopts the spheroidization of the roller, the wall of the roller of the equipment is of a jacket structure, flowing water is introduced into the jacket, the water temperature is controlled at 50 ℃, the rotating speed of the roller is 15r/min, and the spheroidization time is 10 min.
Example 2
Proportioning, mixing and drying
Weighing TiC0.5N0.5 powder: 9.5 kg; 0.4kg of Co powder; fe powder: 0.1kg of polyethylene glycol is added, 50g of polyethylene glycol is added, all the raw materials are uniformly mixed by a ball milling and mixing method, the ball milling agent is alcohol, and then the mixture is obtained by vacuum drying;
② shaping
Sieving by using a 30-mesh sieve for granulation, and then pressing and forming the granulated granules;
thirdly, pre-firing and crushing
Putting the pressed blank prepared in the step II into a vacuum sintering furnace, vacuumizing to below 1 multiplied by 10 < -1 > Pa, heating to 350 ℃, and keeping the temperature for 8 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 800 ℃ for firing for 4 hours; then cooling along with the furnace, and crushing the sintered compact into particles of 30 microns.
Discharge plasma spheroidization
And (4) placing the composite metal ceramic particles prepared in the step (iii) in a radio frequency plasma spheroidizing device which operates stably to spheroidize, so as to obtain the composite metal ceramic spherical powder. The discharge plasma spheroidizing process parameters are as follows: the power is 30KW, the argon working flow is 15slpm, the argon protection flow is 100slpm, the negative pressure of the system is 0.1atm, the powder feeding flow is 2slpm, and the powder feeding speed is 20 g/min. Wherein the temperature of the plasma in the discharge plasma sphering is 3400 ℃.
Example 3
Proportioning, mixing and drying
Weighing (Ti,20W,15Mo,5Ta) C0.7N0.3 powder: 6 kg; co powder: 2.5 kg; 1kg of Ni powder; 0.5kg of Mo powder and 200g of paraffin are uniformly mixed by a ball milling and mixing method, a ball milling agent is acetone, and then the mixture is obtained by vacuum drying;
② shaping
Sieving the mixture by using a sieve of 80 meshes for granulation, and then pressing and forming the granulated granules;
thirdly, pre-firing and crushing
Putting the pressed blank prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas with the air pressure of 500pa in the vacuum furnace, heating to 600 ℃, and keeping the temperature for 2 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1350 ℃ for firing for 0.5 hour; then cooling along with the furnace, and crushing the sintered compact into particles of 100 microns.
Discharge plasma spheroidization
And (4) placing the composite metal ceramic particles prepared in the step (iii) in a radio frequency plasma spheroidizing device which operates stably to spheroidize so as to obtain the composite metal ceramic spherical powder. The discharge plasma spheroidizing process parameters are as follows: the running power is 100KW, the argon working flow is 40slpm, the argon protection flow is 200slpm, the negative pressure of the system is 0.5atm, the powder feeding flow is 8slpm, and the powder feeding speed is 60 g/min. Wherein the temperature of the plasma in the discharge plasma spheroidization is 3600 ℃.
Example 4
Proportioning, mixing and drying
Weighing TiC0.7N0.3 powder: 2 kg; WC:3 kg; mo 2C: 1 kg; 2.7kg of Co powder; ni powder: 1.3kg of butyl rubber, 100g of butyl rubber is added, all the raw materials are uniformly mixed by a ball milling and mixing method, the ball milling agent is acetone, and then the mixture is obtained by vacuum drying;
② shaping
Sieving by a 60-mesh sieve for granulation, and then pressing and forming the granulated granules;
thirdly, pre-firing and crushing
Putting the pressed blank prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas which keeps the air pressure in the vacuum furnace at 1200Pa, heating to 400 ℃, and preserving the heat for 6 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1200 ℃ for firing for 3 hours; then cooling along with the furnace, and crushing the green compact after sintering into particles of 60 microns.
Discharge plasma spheroidization
And (4) placing the composite metal ceramic particles prepared in the step (iii) in a radio frequency plasma spheroidizing device which operates stably to spheroidize so as to obtain the composite metal ceramic spherical powder. The running power is 60KW, the argon working flow is 30slpm, the argon protection flow is 120slpm, the system negative pressure is 0.3atm, the powder feeding flow is 6slpm, and the powder feeding speed is 30 g/min. Wherein the temperature of the plasma in the discharge plasma spheronization is 3900 ℃.
Example 5
Proportioning, mixing and drying
Weighing TiC0.7N0.3 powder: 9.4 kg; MoC: 0.1 kg; 0.5kg of Co powder is added with 300g of SD glue, all the raw materials are uniformly mixed by a ball milling and mixing method, the ball milling agent is acetone, and then the mixture is obtained by vacuum drying;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 300; then, the powder is spheroidized by adopting a roller spheroidizing method, and is sieved by a 30-mesh sieve, and the powder passing through the sieve is taken; sieving with a 50-mesh sieve, and taking the powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the second step into a vacuum sintering furnace, vacuumizing to below 1 x 10 < -1 > Pa, heating to 350 ℃, and keeping the temperature for 8 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 800 ℃ for firing for 4 hours; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process is characterized in that the spheroidization process is carried out by adopting a roller, the wall of the roller is of a two-layer structure and is hollow, the hollow part can be communicated with inflow water, the water temperature is controlled at 50 ℃, the rotating speed of the roller is 15r/min, and the spheroidization time is 10 min.
Example 6
Proportioning, mixing and drying
Weighing (Ti,5W) C0.7N0.3 powder: 9.5 kg; 0.5kg of Ni powder, 400g of paraffin wax is added, the raw materials are uniformly mixed by a ball milling and mixing method, a ball grinding agent is alcohol, and then the mixture is obtained by vacuum drying;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 600 meshes; then, spheroidizing the powder by adopting a roller spheroidizing method, and sieving the powder by using a 100-mesh sieve to obtain the powder passing through the sieve; sieving with 120 mesh sieve, and collecting powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas for keeping the air pressure in the vacuum furnace at 500Pa, heating to 600 ℃, and keeping the temperature for 2 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1300 ℃ for firing for 0.5 hour; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process is characterized in that the spheroidization process is carried out by adopting a roller, the wall of the roller is of a two-layer structure and is hollow, water can be introduced into the hollow part, the water temperature is controlled at 80 ℃, the rotating speed of the roller is 45r/min, and the spheroidization time is 20 min.
Example 7
Proportioning, mixing and drying
Weighing (Ti,20W,15Mo,5Ta) C0.5N0.5 powder: 4.65 kg; 0.25kg of TiCN; 2kg of WC; MoC: 1 kg; 1kg of TaC; 0.1kg of NbC; 1kg of Mo powder; adding 350g of polyethylene glycol, uniformly mixing the raw materials by a ball milling and mixing method, wherein a ball milling agent is alcohol, and then drying in vacuum to obtain a mixture;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 600 meshes; then, spheroidizing the powder by adopting a roller spheroidizing method, and sieving the powder by using a 100-mesh sieve to obtain the powder passing through the sieve; sieving with 120 mesh sieve, and collecting powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas for keeping the air pressure in the vacuum furnace at 1200Pa, heating to 600 ℃, and keeping the temperature for 2 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1300 ℃ for firing for 0.5 hour; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process is characterized in that the spheroidization process is carried out by adopting a roller, the wall of the roller is of a two-layer structure and is hollow, water can be introduced into the hollow part, the water temperature is controlled at 80 ℃, the rotating speed of the roller is 45r/min, and the spheroidization time is 20 min.
Example 8
Proportioning, mixing and drying
Weighing 2kg of (Ti,5Cr,2V,0.2Nb) C0.3N0.7 powder; 1.5kg of WC powder; 0.5kg of Cr3C 2; VC accounts for 0.5 kg; 1kg of TaC powder; 0.5kg of NbC; 1.8kg of Co powder; 1.8kg of Ni powder; 0.4kg of Fe powder, adding 200g of paraffin, uniformly mixing the raw materials by a ball milling and mixing method, and taking out to obtain mixed slurry;
② spray granulation
Carrying out spray granulation treatment on the slurry obtained in the step I by adopting a high-speed centrifugal spray granulation dryer so as to obtain spherical powder; the fog granulation process comprises setting inlet temperature at 100 deg.C, outlet temperature at 80 deg.C, atomizer rotation speed at 10kr/min, and slurry input speed at 5 ml/min;
(iii) Heat treatment
Placing the spherical powder obtained in the second step in a vacuum sintering furnace for heat treatment, wherein the heating rate is 3 ℃/min, the heat treatment temperature is 800 ℃, and the heat treatment time is 5 hours; and then cooling to room temperature along with the furnace to obtain the spherical powder of the metal ceramic composite alloy.
Example 9
Proportioning, mixing and drying
9.4kg of (Ti,10W, 5Mo,1Zr) C0.7N0.3 powder is weighed; 0.1kg of ZrC; 0.5kg of Co powder is added with 90g of SD glue, all the raw materials are uniformly mixed by a ball milling and mixing method, and the mixture is taken out to obtain mixed slurry;
② spray granulation
Carrying out spray granulation treatment on the slurry obtained in the step I by adopting a high-speed centrifugal spray granulation dryer so as to obtain spherical powder; the fog granulation process comprises setting inlet temperature at 350 deg.C, outlet temperature at 250 deg.C, atomizer rotation speed at 25kr/min, and slurry input speed at 22 ml/min;
(iii) Heat treatment
Placing the spherical powder obtained in the second step in a vacuum sintering furnace for heat treatment, wherein the heating rate is 10 ℃/min, the heat treatment temperature is 1300 ℃, and the heat treatment time is 0.5 h; and then cooling to room temperature along with the furnace to obtain the spherical powder of the metal ceramic composite alloy.
Example 10
Proportioning, mixing and drying
Weighing 0.095kg of TiC0.7N0.3 powder; (Ti,10W,5Ta) C0.3N0.7:0.005 kg; 3kg of WC; 1.5kg of Mo2C powder; 1kg of TaC powder; 1kg of Cr3C2 powder; 0.5kg of VC powder; 2kg of Fe powder; 0.9kg of Ni powder; adding 400g of SD (secure digital) glue, uniformly mixing the raw materials by a ball milling and mixing method, wherein a ball milling agent is acetone, and then drying in vacuum to obtain a mixture;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 300; then, the powder is spheroidized by adopting a roller spheroidizing method, and is sieved by a 60-mesh sieve, and the powder passing through the sieve is taken; sieving with 80 mesh sieve, and collecting powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the step II into a vacuum sintering furnace, vacuumizing to below 1 x 10 < -1 > Pa, heating to 450 ℃, and keeping the temperature for 5 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1000 ℃ for firing for 3 hours; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process is characterized in that the spheroidization process is carried out by adopting a roller, the wall of the roller is of a two-layer structure and is hollow, the hollow part can be communicated with inflow water, the water temperature is controlled at 50 ℃, the rotating speed of the roller is 15r/min, and the spheroidization time is 10 min.
Example 11
Proportioning, mixing and drying
3kg of TiC0.7N0.3 powder is weighed; (Ti,10W,8Mo) C0.5N0.5:1 kg; WC:3 kg; mo 2C: 2 kg; 1kg of Fe powder; adding 450g of buna rubber, uniformly mixing the raw materials by a ball milling and mixing method, wherein a ball milling agent is acetone, and then drying in vacuum to obtain a mixture;
② shaping
Sieving the mixture by using a 60-mesh sieve for granulation, and then pressing and forming the granulated granules;
thirdly, pre-firing and crushing
Putting the pressed blank prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas which keeps the air pressure in the vacuum furnace at 1200Pa, heating to 400 ℃, and preserving the heat for 6 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1200 ℃ for firing for 3 hours; then cooling along with the furnace, and crushing the green compact after sintering into particles of 60 microns.
Discharge plasma spheroidization
And (4) placing the composite metal ceramic particles prepared in the step (iii) in a radio frequency plasma spheroidizing device which operates stably to spheroidize so as to obtain the composite metal ceramic spherical powder. The running power is 60KW, the argon working flow is 30slpm, the argon protection flow is 120slpm, the system negative pressure is 0.3atm, the powder feeding flow is 6slpm, and the powder feeding speed is 30 g/min. Wherein the temperature of the plasma in the discharge plasma spheroidization is 3200 ℃.
Example 12
Proportioning, mixing and drying
Weighing 8kg of (Ti,5W) C0.7N0.3 powder; 2kg of Fe powder, adding 500g of paraffin, uniformly mixing the raw materials by a ball milling and mixing method, wherein a ball milling agent is alcohol, and then drying in vacuum to obtain a mixture;
② spheroidization
Crushing, sieving and powdering the mixture prepared in the step I, wherein the number of the sieving meshes is 600 meshes; then, spheroidizing the powder by adopting a roller spheroidizing method, and sieving the powder by using a 90-mesh sieve to obtain the powder passing through the sieve; sieving with 100 mesh sieve, and collecting powder which does not pass through the sieve to obtain spherical powder with uniform particle size distribution;
removing forming agent and heat treatment
Putting the spherical powder prepared in the step II into a vacuum sintering furnace, continuously introducing flowing Ar gas for keeping the air pressure in the vacuum furnace at 500Pa, heating to 600 ℃, and keeping the temperature for 2 hours to remove the added forming agent; then reducing the air pressure to below 1 x 10 < -1 > Pa, and then heating to 1300 ℃ for firing for 0.5 hour; then cooling along with the furnace to obtain spherical powder of the metal ceramic composite alloy;
the spheroidization process is characterized in that the spheroidization process is carried out by adopting a roller, the wall of the roller is of a two-layer structure and is hollow, water can be introduced into the hollow part, the water temperature is controlled at 80 ℃, the rotating speed of the roller is 35r/min, and the spheroidization time is 20 min.
Claims (7)
1. Based on (Ti, Me) CN-MxThe coating spraying and 3D printing cermet material of C-Co is characterized in that the cermet material is spherical powder, and comprises the following components in percentage by mass: (Ti, Me) CN-MxC-Co and at least one selected from Ni, Mo and Fe, the content of (Ti, Me) CN is 20-94%, MxThe content of C is 1-40%, and the content of Co and at least one of Ni, Mo and Fe is 5-40%; the metal Me is at least one of W, Mo, Ta, V, Cr, Nb and Zr; carbide MxC of WC, TaC and Cr3C2NbC and VC; me in the (Ti, Me) CN accounts for 5-40% of the total mass of the Ti and the Me; prepared by a method comprising the following process steps:
(1) mixing and drying, namely adding the raw material powder and a ball milling agent in a formula amount into ball milling mixing equipment, fully ball milling and mixing to obtain a mixture, and fully drying the obtained mixture in drying equipment to obtain a dried mixture;
(2) spheroidizing powder, namely crushing the dried mixture obtained in the step (1), sieving the crushed mixture by using a 300-600-mesh sieve, feeding the sieved powder material into a spheroidizing roller to spheroidize the powder, and sieving the spheroidized powder to remove the spheroidized powder with the particle size of more than 30 meshes and less than 120 meshes, thereby obtaining the spheroidized powder with uniform particle size distribution;
and adding a forming agent before granulation;
(3) sintering treatment, namely putting the spherical powder prepared in the step (2) into a vacuum sintering furnace, and vacuumizing to 1 × 10-1Keeping the air pressure in the vacuum sintering furnace at 500-1200 Pa below Pa or continuously introducing Ar gas, heating to 350-600 ℃, keeping the temperature for 2-8 hours to remove the added forming agent, and then carrying out vacuum 1 × 10-1Heating to 800-1300 ℃ below Pa, firing for 0.5-4 hours, and cooling along with the furnace to obtain the metal ceramic composite alloy ballForming powder;
or prepared by a method comprising the following process steps:
(1) mixing and drying, namely adding the raw material powder and the ball milling agent in a formula amount into ball milling mixing equipment, fully ball milling and mixing to obtain a mixture, and fully drying the obtained mixture in drying equipment to obtain a dried mixture;
(2) pressing and forming, namely sieving and granulating the mixture prepared in the step (1) by using a 30-80-mesh sieve, and then pressing and forming the sieved granules;
and adding a forming agent before granulation;
(3) firing and crushing, namely putting the formed blank obtained in the step (2) into a vacuum sintering furnace, and vacuumizing to 1 × 10-1Keeping the air pressure in the vacuum sintering furnace at 500-1200 Pa below Pa or continuously introducing Ar gas, heating to 350-600 ℃, keeping the temperature for 2-8 hours to remove the forming agent, and then carrying out vacuum 1 × 10-1Heating to 800-1300 ℃ below Pa, firing for 0.5-4 hours, cooling along with the furnace, and crushing the sintered formed blank into 30-100 micron particles;
(4) performing radio frequency plasma spheroidization, namely placing the granular material with the grain size of 30-100 microns obtained in the step (3) in a radio frequency plasma spheroidizing device for spheroidization under the protection of argon to obtain spherical powder of the metal ceramic composite alloy;
or prepared by a method comprising the following process steps:
(1) mixing and drying, namely adding the raw material powder, the ball grinding agent and the forming agent in the formula ratio into ball-milling mixing equipment, and fully ball-milling and mixing to obtain mixed slurry;
(2) spray granulation, namely feeding the slurry obtained in the step (1) into a centrifugal spray granulation dryer for spray granulation to obtain spherical powder;
(3) and (3) sintering heat treatment, namely placing the spherical powder obtained in the step (2) in a vacuum sintering furnace, heating to 800-1300 ℃ at the heating rate of 3-10 ℃/min, sintering for 0.5-5 h, and then cooling to room temperature along with the furnace to obtain the spherical powder of the metal ceramic composite alloy.
2. (Ti, M) -based according to claim 1e)CN-MxThe coating spraying and 3D printing cermet material of C-Co is characterized in that a ball grinding agent added in the process of preparing mixed slurry by ball milling and mixing is alcohol or acetone.
3. (Ti, Me) -based CN-M according to claim 1xThe coating spraying and 3D printing cermet material of C-Co is characterized in that the forming agent is one of polyethylene glycol, paraffin, buna rubber and SD rubber, and the addition amount of the forming agent is 0.5-5% of the total mass of the raw material powder.
4. (Ti, Me) -based CN-M according to claim 1 or 2 or 3xThe coating spraying and 3D printing cermet material of C-Co is characterized in that a sphericizing roller is adopted for powder sphericizing, the wall of the roller is of a jacket structure, circulating water flow with the temperature of 50-80 ℃ is introduced into the jacket, the rotating speed of the roller is 15-45 r/min, and the sphericizing time is 10-20 min.
5. (Ti, Me) -based CN-M according to claim 1 or 2 or 3xThe C-Co coating spraying and 3D printing metal ceramic material is characterized in that the operation power of a radio frequency plasma spheroidizing device is 30-100 KW, the argon working flow is 15-40 slpm, the argon protection flow is 100-200 slpm, the negative pressure of a system is 0.1-0.5 atm, the powder feeding gas flow is 2-8 slpm, and the powder feeding speed is 20-60 g/min.
6. (Ti, Me) -based CN-M according to claim 5xThe coating spraying and 3D printing cermet material of C-Co is characterized in that the temperature of discharge plasma of the radio frequency plasma spheroidizing device is not lower than 3200 ℃.
7. (Ti, Me) -based CN-M according to claim 1 or 2 or 3xThe coating spraying and 3D printing metal ceramic material of C-Co is characterized in that the operating inlet temperature of the centrifugal spray granulation dryer is 100-350 ℃, the outlet temperature is 80-250 ℃, the rotating speed is 10-25 kr/min, and the slurry feeding speed is 5-22 ml/min.
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| CN108213410A (en) | 2018-06-29 |
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| CN106270493A (en) | 2017-01-04 |
| CN108213411B (en) | 2020-08-25 |
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| CN106270493B (en) | 2020-06-30 |
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