CN115519126A - Optimization method of high-sphericity titanium alloy and ceramic reinforcement composite powder ball-milling powder mixing process - Google Patents
Optimization method of high-sphericity titanium alloy and ceramic reinforcement composite powder ball-milling powder mixing process Download PDFInfo
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Abstract
The invention relates to a ball milling and powder mixing process optimization method for high sphericity titanium alloy and ceramic reinforcement composite powder, which comprises the step of shooting a micro-scanning picture of the composite powder of the titanium alloy and the ceramic reinforcement obtained under the ball milling and powder mixing process parameters to be optimized; and calculating the deformation rate omega of the composite powder particles in the field of view of the micro-scanning photo, and finally, taking the corresponding process parameter with the deformation rate lower than 10 percent as the optimized ball-milling powder mixing process parameter. The method optimizes the technological parameters of the ball milling and powder mixing of the titanium alloy composite powder based on the sphericity Q and the deformation rate omega of the composite powder individual after the ball milling and powder mixing, prepares the titanium alloy composite powder with high sphericity by using the optimized technological parameters, facilitates the industrial application, and reduces the manpower and material resources; meanwhile, the optimization process can be applied to the ball-milling powder mixing process of other alloy or ceramic reinforcement bodies.
Description
Technical Field
The invention relates to the technical field of metal powder manufacturing, in particular to a preparation technology of high-sphericity titanium alloy and reinforcement composite powder.
Background
The titanium alloy has high specific strength, high toughness, good fatigue resistance, creep resistance, corrosion resistance and the like, and is mainly used for manufacturing parts of a gas compressor of an aeroengine, such as parts of blades, gas compressor disks, engine brakes and the like, and key structural parts of rockets, missiles and high-speed aircrafts; the method is also widely applied to the fields of electrolysis, power stations, petroleum, seawater desalination, environmental pollution control and the like. However, further improvements are needed to meet the more severe service conditions based on their superior overall performance. At present, the maximum service temperature of the high-temperature titanium alloy is 600 ℃, and in order to meet the service requirements of high temperature resistance and high toughness of a titanium alloy component, the high-temperature mechanical property and the service temperature of the titanium alloy need to be further improved. Research shows that the titanium-based composite material prepared by the in-situ self-generated enhanced phase method is one of effective ways for solving the problem.
Since the physical properties of titanium alloy composite powders, such as particle size and sphericity, directly affect the properties of titanium-based composites and components, in-situ self-formation of titanium-based composites places severe demands on the alloy powders. The preparation method of the titanium alloy composite powder is a ball milling and powder mixing method which enables different alloy powders to be combined more uniformly by a physical extrusion method under a certain ball milling condition.
The preparation method of the ball-milling mixed powder adopting the composite powder can provide raw materials for the preparation of the titanium-based composite material and the additive manufacturing of the titanium-based composite material component, and is effectively applied to the manufacturing of key components in the aerospace field. Document 1, A.Tang, L.J.Huang, X.D.Rong, et al. Effects of volume fractions on the microstructure and mechanical properties of TiBw/Ti compositions [ J.]Acta materials composition Sinica,2013,30 "discloses a TiB composition comprising 2 And Ti powder, wherein the ball milling rotation speed is 250r/min, the ball-to-material ratio is 5:1, tiB is obtained under the condition that the ball milling time is 11h 2 A Ti alloy composite powder.
In the process of ball-milling and mixing the titanium alloy and reinforcement composite powder, if the composite powder loses the spherical shape and becomes flat, the mechanical property of the prepared titanium-based composite material or the manufactured titanium-based composite material member can not meet the requirement. Meanwhile, the powder is mixed by ball milling of the titanium alloy and the reinforcement composite powder under the condition of no protective atmosphere, and the powder is likely to react with oxygen in the air, so that the titanium alloy and the reinforcement composite powder are oxidized, and the mechanical property of the prepared titanium-based composite material or the manufactured titanium-based composite material member can not meet the requirement.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides the optimization method of the high-sphericity titanium alloy and ceramic reinforcement composite powder ball-milling powder mixing process, which is based on the fact that the ball-milling powder mixing meets the powder sphericity and the deformation rate, so as to obtain the optimized process parameters of the composite powder ball-milling powder mixing.
In order to achieve the purpose, the invention adopts the technical scheme that: a ball-milling powder mixing process optimization method for high-sphericity titanium alloy and ceramic reinforcement composite powder comprises the following steps:
step one, taking composite powder of a titanium alloy and a ceramic reinforcement obtained under ball-milling powder mixing process parameters to be optimized, flatly paving and adhering the composite powder on conductive adhesive, randomly selecting composite powder areas on at least 3 conductive adhesives, and respectively scanning each area by a micro scanning picture of 70-100 times or less;
step two, marking at least one layer of ceramic reinforcement powder particles adhered in the field of view of the micro-scanning picture as single composite powder particles, and counting the total number of the single composite powder particles in the micro-scanning picture as N 2 And the number of individual composite powder particles losing the spherical shape is recorded as N 1 The single composite powder particle losing the spherical shape refers to a particle having a single sphericity Q of less than 0.7, and the deformation rate ω of the composite powder particle is calculated by the formula:
and step three, taking the corresponding technological parameter with the deformation rate lower than 10% as the optimized ball-milling powder-mixing technological parameter.
Further, the single sphericity Q in the second step is to take any single composite powder particle in the field of view of the micro-scanning picture, draw a maximum inscribed circle and a minimum circumscribed circle of the particle, arbitrarily take two chords on the circle, wherein the circle center is the intersection point of the perpendicular bisectors of the two chords, and the radius is any distance from the circle center to the circumference; calculating the individual sphericity Q of the individual composite powder particles, the calculation formula of the individual sphericity Q being represented as:
in the formula: r is a radical of hydrogen 1 Is the maximum inscribed circle radius of the composite powder, and the unit is mum; r is 2 Is the minimum circumscribed circle radius of the composite powder, and has a unit of μm;
when the sphericity is 1, the single composite powder particle is a strictly spherical particle; when the sphericity is less than 0.7, the single composite powder particle is a single composite powder particle which loses the spherical shape, the fluidity of the single composite powder particle which loses the spherical shape is reduced, and the number of reflections of light is reduced; and after the sphericity calculation of all the single composite powder particles in the field of view of the micro-scanning photo is finished, starting to calculate the deformation rate of the composite powder particles.
Further, the ball milling and powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps:
(a) Putting the mixed powder of spherical titanium alloy particles and ceramic reinforcement required to be optimized and stainless steel grinding balls into a ball milling tank, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of that of the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement required to be optimized, when the mass ratio of the ceramic reinforcement particles is increased, the ball milling speed is required to be increased, the ball milling time is required to be prolonged, the sphericity of the composite powder particles is reduced, and the deformation rate is increased; the mass ratio of the stainless steel grinding balls to the mixed powder is (4-5) to 1, the spherical titanium alloy particles are mixed particles with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, and the mass ratio of the corresponding mixed particles is (1-2) to (3-4) to (6-8);
(b) Performing ball milling and powder mixing on the composite powder on a planetary ball mill, setting the ball milling time to be 4-10 h, the ball milling rotating speed to be 200-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotation for 60-70 min along the same direction and stopping for 5-10 min; the forward and reverse rotation means that the material rotates forwards for 25-35 min, stops for 5-10 min and rotates reversely for 25-35 min;
(c) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h and opening the ball milling tank to take out 1-2 g of powder to perform the optimization method to obtain a group of observation data of sphericity and deformability, continuing to perform ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, wherein the total time of ball milling and powder mixing is 7-10 h, taking out at least 3-6 groups in sequence to observe, and correspondingly obtaining the observation data of sphericity and deformability.
Further, the ball milling and powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps:
(a) Mixing spherical titanium alloy particles to be optimized and ceramic reinforcement mixed powder, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of that of the spherical titanium alloy particles to be optimized and the ceramic reinforcement mixed powder, and taking stainless steel grinding balls with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, wherein the mass ratio of the stainless steel grinding balls to the mixed powder is (4-5): 1, the mass ratio of the corresponding mixed particles is (1-2) to (3-4) to (6-8);
(b) Putting the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and stainless steel grinding balls into a ball milling tank, vacuumizing, introducing argon at the speed of 2-3L/s for 2-3 s when the vacuum degree reaches- (0.1-0.2) MPa, and repeating the process for at least 2-3 times;
(c) Placing a ball milling tank in a vacuum state in a planetary ball mill, setting the rotation speed to be 300-400 rpm, setting the ball milling direction to be one-way, rotating for 1-2 hours each time, staying for 5-10 minutes, ensuring the total rotation time to be 5-10 hours, stopping rotating the planetary ball mill every 1 hour, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method to obtain a group of observed sphericity and deformation data, continuing performing ball milling and powder mixing on the powder in the ball milling tank after 5-10 minutes, setting the total ball milling and powder mixing time to be 7-10 hours, taking out at least 3-6 groups successively for observation, and correspondingly obtaining the sphericity and deformation observation data.
Further, the concrete process of laying and adhering the composite powder on the conductive adhesive in the first step is as follows: shearing 5 multiplied by 15mm conductive adhesive, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a 5 multiplied by 8mm area on the conductive adhesive, spreading 0.5-1 g of composite powder in the area, blowing off the composite powder which is not adhered to the conductive adhesive by using an ear blowing ball, and blowing for at least 10 times.
Furthermore, the statistical software used in the second step is Image J software.
And further, utilizing the ball milling powder mixing deformation rate omega in the step two to list the deformation single composite powder particle number and deformation rate influence table corresponding to the titanium alloy and ceramic reinforcement powder mixing process parameters, thereby realizing the optimization of the titanium alloy and ceramic reinforcement powder mixing process parameters.
Furthermore, the titanium alloy particles are titanium alloy particles with spherical morphology, and the ceramic reinforcement particles are non-spherical morphology particles with adhesion capability.
The invention has the beneficial effects that: the method optimizes the technological parameters of the ball milling and powder mixing of the titanium alloy composite powder based on the sphericity Q and the deformation rate omega of the composite powder individual after the ball milling and powder mixing, prepares the titanium alloy composite powder with high sphericity by using the optimized technological parameters, facilitates the industrial application, and reduces the manpower and material resources; meanwhile, the optimized process can be applied to the ball-milling powder mixing process of other alloy or ceramic reinforcement bodies.
Drawings
FIG. 1 is 5wt% TiB 2 The individual powder sphericity quantitative schematic diagram of the/Ti 6242 alloy composite powder;
FIG. 2 is 5wt% TiB at a rotation speed of 300r/min for a total rotation time of 8h 2 Microstructure photograph of the/Ti 6242 composite powder;
FIG. 3 shows the 5wt% TiB at a rotation speed of 300r/min for a total rotation time of 9h 2 Microstructure photograph of the/Ti 6242 composite powder;
FIG. 4 is 5wt% TiB at a rotation speed of 300r/min for a total rotation time of 10h 2 Microstructure photograph of the/Ti 6242 composite powder;
FIG. 5 is 5% by weight of TiB at a rotation speed of 400r/min for a total rotation time of 5h 2 Microstructure photograph of the/Ti 6242 composite powder;
FIG. 6 shows the 5wt% TiB at a rotation speed of 400r/min for a total rotation time of 6h 2 Microstructure photograph of the/Ti 6242 composite powder;
FIG. 7 shows the 5wt% TiB at a rotation speed of 400r/min for a total rotation time of 7h 2 Microstructure photograph of the/Ti 6242 composite powder.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
In order to achieve the above object, the present invention provides the following embodiments:
example 1: a ball-milling powder mixing process optimization method for high-sphericity titanium alloy and ceramic reinforcement composite powder comprises the following steps:
step one, taking composite powder of titanium alloy and ceramic reinforcement obtained under the ball milling powder mixing process parameters to be optimized, flatly paving and adhering the composite powder on conductive adhesive, randomly selecting at least 3 composite powder areas on the conductive adhesive, and respectively scanning each area by a micro scanning picture of 70-100 times or less; the concrete process of the compound powder tiled and adhered on the conductive adhesive comprises the following steps: cutting off 5 multiplied by 15mm conductive adhesive, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a 5 multiplied by 8mm area on the conductive adhesive, spreading 0.5-1 g of composite powder in the area, blowing off the composite powder which is not adhered to the conductive adhesive by using an ear blowing ball, and blowing for at least 10 times.
Step two, marking at least one layer of ceramic reinforcement powder particles adhered in the field of view of the micro-scanning picture as single composite powder particles, and counting the total number of the single composite powder particles in the micro-scanning picture as N 2 And the number of individual composite powder particles losing the spherical shape is recorded as N 1 The single composite powder particle losing the spherical shape is referred to as a single particleParticles with sphericity Q less than 0.7, and calculating the deformation rate omega of the composite powder particles by the formula:
the single sphericity Q is obtained by taking any single composite powder particle in the field of view of the micro-scanning picture, drawing a maximum inscribed circle and a minimum circumscribed circle of the particle, taking any two chords on the circle, wherein the circle center is the intersection point of the vertical bisectors of the two chords, and the radius is the distance from the circle center to any point of the circumference; calculating the individual sphericity Q of the individual composite powder particles, the calculation formula of the individual sphericity Q being represented as:
in the formula: r is 1 -the maximum inscribed circle radius of the composite powder in μm; r is 2 -the minimum circumscribed circle radius of said composite powder in μm;
when the sphericity is 1, the single composite powder particle is a strictly spherical particle; when the sphericity is less than 0.7, the single composite powder particle is a single composite powder particle which loses the spherical shape, the fluidity of the single composite powder particle which loses the spherical shape is reduced, and the number of reflections of light is reduced; and after the calculation of the sphericity of all the single composite powder particles in the field of view of the micro-scanning photo is finished, the deformation rate of the composite powder particles is calculated.
The statistical software of the composite powder particle deformation rate omega is Image J software.
And step three, taking the corresponding technological parameter with the deformation rate lower than 10% as the optimized technological parameter for ball milling and powder mixing. And listing the number of deformed single composite powder particles and a deformation rate influence table corresponding to the technological parameters of the mixed powder of the titanium alloy and the ceramic reinforcement by using the ball-milling mixed powder deformation rate omega in the step two, thereby realizing the optimization of the technological parameters of the mixed powder of the titanium alloy and the ceramic reinforcement.
The ball-milling powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps of:
(a) Putting the mixed powder of spherical titanium alloy particles and ceramic reinforcements to be optimized and stainless steel grinding balls into a ball milling tank, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of the mass of the mixed powder of the spherical titanium alloy particles and the ceramic reinforcements to be optimized, the mass ratio of the stainless steel grinding balls to the mixed powder is (4-5): 1, the spherical titanium alloy particles are mixed particles with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, and the mass ratio of the corresponding mixed particles is (1-2): (3-4): (6-8);
(b) Performing ball milling and powder mixing on the composite powder on a planetary ball mill, setting the ball milling time to be 4-10 h, the ball milling rotating speed to be 200-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotation for 60-70 min along the same direction and stopping for 5-10 min; the forward and reverse rotation means forward rotation for 25-35 min, stop for 5-10 min and reverse rotation for 25-35 min;
(c) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h and opening the ball milling tank to take out 1-2 g of powder to perform the optimization method to obtain a group of observation data of sphericity and deformability, continuing to perform ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, wherein the total time of ball milling and powder mixing is 7-10 h, taking out at least 3-6 groups in sequence to observe, and correspondingly obtaining the observation data of sphericity and deformability.
The titanium alloy particles are spherical titanium alloy particles, the ceramic reinforcement particles are non-spherical particles with adhesive capacity, the mass of the ceramic reinforcement particles accounts for 1-7% of the total mass of the mixed powder of the initial titanium alloy particles and the ceramic reinforcement particles, when the mass ratio of the ceramic reinforcement particles is increased, the ball milling speed needs to be increased, the ball milling time needs to be prolonged, the sphericity of the composite powder particles is reduced, and the deformation rate is increased.
Example 2: the same as in example 1, except that: the ball-milling powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps of:
(a) Mixing spherical titanium alloy particles to be optimized and ceramic reinforcement mixed powder, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of that of the spherical titanium alloy particles to be optimized and the ceramic reinforcement mixed powder, and taking stainless steel grinding balls with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, wherein the mass ratio of the stainless steel grinding balls to the mixed powder is (4-5): 1, the mass ratio of the corresponding mixed particles is (1-2) to (3-4) to (6-8);
(b) Putting the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and stainless steel grinding balls into a ball milling tank, vacuumizing, introducing argon at the speed of 2-3L/s for 2-3 s when the vacuum degree reaches- (0.1-0.2) MPa, and repeating the process for at least 2-3 times;
(c) Placing a ball milling tank in a vacuum state in a planetary ball mill, setting the rotation speed to be 300-400 rpm, setting the ball milling direction to be one-way, rotating for 1-2 hours each time, staying for 5-10 minutes, ensuring the total rotation time to be 5-10 hours, stopping rotating the planetary ball mill every 1 hour, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method to obtain a group of observed sphericity and deformation data, continuing performing ball milling and powder mixing on the powder in the ball milling tank after 5-10 minutes, setting the total ball milling and powder mixing time to be 7-10 hours, taking out at least 3-6 groups successively for observation, and correspondingly obtaining the sphericity and deformation observation data.
The invention is suitable for the mixed powder of titanium alloy particles with spherical morphology and ceramic reinforcement particles with non-spherical morphology and adhesive capacity, the titanium alloy mainly relates to Ti6242 particles or Ti6Al4V particles, and the ceramic reinforcement can be TiB 2 Powder particles or TiC powder particles, the invention will now be further described by means of experimental examples.
Experimental example 1: as shown in FIGS. 1-7, the ceramic reinforcement used in this example was TiB 2 The method comprises the following steps of:
(1) Weighing the components in a mass ratio of 1: tiB of 19 2 Powder particles and Ti6242 powder particles, balanceTaking stainless steel grinding balls with the diameters of 5mm, 8mm and 10mm respectively, wherein the mass ratio of powder to the grinding balls is 1:5, the mass ratio of the grinding balls with different diameters is 6:3:1;
(2) Mixing weighed Ti6242 powder particles with 5wt% 2 Putting the powder particles and stainless steel grinding balls into a vacuum grinding tank, vacuumizing, introducing argon at the speed of 2L/s for 2s when the vacuum degree reaches-0.1 MPa, and repeating the process for 3 times;
(3) Placing the vacuum ball milling tank in a planetary ball mill, setting the rotation speed to be 300r/min or 400r/min, setting the ball milling direction to be one-way, rotating for 1 hour each time, and staying for 10 minutes, wherein the total rotation time is 5-10 hours; stopping rotating the planetary ball mill every 1h, opening a ball milling tank, taking out 1-2 g of powder, performing the optimization method to obtain a group of observed sphericity and deformation data, continuing performing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, wherein the total ball milling and powder mixing time is 7-10 h, taking out at least 6 groups in sequence for observation, and correspondingly obtaining the sphericity and deformation observation data;
(4) Observing the 6 groups selected in the step 3, and taking 3 micro-scanning pictures of different areas under 70 times for each group;
(5) Drawing in the field of view of a microscopic scanning photograph at least one layer of ceramic reinforcement powder particles adhered thereto as individual Ti6242 and 5wt% 2 Drawing a maximum inscribed circle and a minimum circumscribed circle of a single composite powder particle, arbitrarily taking two chords on the circle, wherein the circle center is the intersection point of perpendicular bisectors of the two chords, and the radius is any distance from the circle center to the circumference;
calculating individual Ti6242 and 5wt% TiB 2 The sphericity Q of the composite powder particles is represented by the calculation formula:
in the formula: q-individual Ti6242 and 5wt% TiB 2 Sphericity of the composite powder;
r 1 -Ti 6242 and 5wt% -TiB 2 Maximum inscribed circle radius (μm) of the composite powder;
r 2 -Ti 6242 and 5wt% TiB 2 Minimum circumscribed circle radius (μm) of the composite powder.
When the sphericity is 1, single Ti6242 and 5wt% TiB 2 The composite powder is strictly spherical particles, ti6242 and 5wt% TiB 2 The sphericity of the composite powder meets the requirement; when the sphericity is less than 0.7, single Ti6242 and 5wt% 2 The composite powder was a composite powder lost in spherical shape, and the calculation of Ti6242 and 5wt% of TiB was continued 2 Deformation rate of the composite powder. After the calculation of the sphericity of all the single composite powder particles in the field of view of the 6 groups of the micro-scanning photographs is completed, the calculation of the deformation rate of the composite powder particles is started.
(6) Statistics of Ti6242 and 5wt% in each photograph Using Image J software 2 Total number of composite powders, calculated loss of spherical shape Ti6242 and 5wt% TiB in all the micrographs 2 Number of particles N of composite powder 1 Counting Ti6242 and TiB with sphericity Q less than 0.7 in each microscopic scanning picture 2 The amount of the composite powder calculated to Ti6242 and 5wt% of TiB in all photographs 2 The total number of particles N2 of the composite powder;
calculating Single Ti6242 and 5wt% 2 Characterization method of composite powder deformation rate omega. The deformation ratio means the contents of Ti6242 and 5wt% of the ball-shaped loss of TiB 2 The number of composite powder particles and Ti6242 and 5wt% 2 The percentage of the total number of composite powder particles, i.e. the deformation ratio ω, is calculated by the formula:
in the formula: n is a radical of 1 Irregular Ti6242 and 5wt% of loss of sphericity in all photographs TiB 2 The number of composite powder particles;
N 2 ti6242 and 5wt% of TiB in all photographs 2 Total number of composite powder particles.
When the deformation is higher than 10%, the process parameters are stated as Ti6242 and 5wt% TiB 2 Low sphericity of the composite powder, ti6242 and 5wt% 2 Composite powderDoes not meet the requirements.
(7) Finally, according to the calculated deformation rate omega, the process parameters corresponding to the deformation rate lower than 10 percent are taken as the optimized ball-milling powder mixing process parameters, so that the optimized Ti6242 and 5wt% of TiB are realized 2 A ball milling and powder mixing process of composite powder.
Different process parameters to obtain Ti6242 and 5wt% TiB 2 The results of the calculation of the composite powder deformation ratio ω are shown in table 1. According to Table 1, preferably Ti6242 and 5wt% 2 The technological parameters of the ball milling and powder mixing of the composite powder are as follows: the ball milling speed is 300r/min, and the total ball milling time is 8h.
TABLE 1 deformation rate values of Ti6242 and 5wt%
| Ball milling speed (r/min) | 300 | 300 | 300 | 400 | 400 | 400 |
| Ball milling time (h) | 8 | 9 | 10 | 5 | 6 | 7 |
| Total number of particles (one) | 3088 | 5234 | 3870 | 2380 | 2713 | 2491 |
| Number of deformation particles | 44 | 87 | 78 | 121 | 292 | 402 |
| Percent deformation (%) | 1.42 | 1.66 | 2.01 | 5.08 | 10.76 | 16.14 |
According to the invention, the sphericity Q and the deformation rate omega of the composite powder after ball milling and powder mixing are taken as the basis, the ball milling and powder mixing technological parameters of the titanium alloy composite powder are optimized, the titanium alloy composite powder with high sphericity is prepared by using the optimized technological parameters, the industrial application is facilitated, and the manpower and material resources are reduced.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A ball milling and powder mixing process optimization method for high-sphericity titanium alloy and ceramic reinforcement composite powder is characterized by comprising the following steps:
step one, taking composite powder of titanium alloy and ceramic reinforcement obtained under the ball milling powder mixing process parameters to be optimized, flatly paving and adhering the composite powder on conductive adhesive, randomly selecting at least 3 composite powder areas on the conductive adhesive, and respectively scanning each area by a micro scanning picture of 70-100 times or less;
marking at least one layer of ceramic reinforcement powder particles adhered in the microscopic scanning photograph view field as single composite powder particles, and counting the total number of the single composite powder particles in the microscopic scanning photograph as N 2 And the number of individual composite powder particles losing the spherical shape is recorded as N 1 The single composite powder particle losing the spherical shape refers to a particle having a single sphericity Q of less than 0.7, and the deformation rate ω of the composite powder particle is calculated by the formula:
and step three, taking the corresponding technological parameter with the deformation rate lower than 10% as the optimized technological parameter for ball milling and powder mixing.
2. The optimization method for the ball-milling powder mixing process of the high sphericity titanium alloy and the ceramic reinforcement composite powder according to claim 1, wherein in the second step, the single sphericity Q is obtained by taking any single composite powder particle in the view field of the micro-scanning photograph, drawing a maximum inscribed circle and a minimum circumscribed circle of the particle, and taking any two chords on the circle, wherein the center of the circle is the intersection point of vertical bisectors of the two chords, and the radius is the distance from the center of the circle to any point of the circumference; calculating the individual sphericity Q of the individual composite powder particles, the individual sphericity Q being calculated by the formula:
in the formula: r is a radical of hydrogen 1 Is the maximum inscribed circle radius of the composite powder, and the unit is mum; r is a radical of hydrogen 2 Is the minimum circumscribed circle radius of the composite powder, and has a unit of mu m;
when the sphericity is 1, the single composite powder particle is a strictly spherical particle; when the sphericity is less than 0.7, the single composite powder particle is a single composite powder particle which loses the spherical shape, the fluidity of the single composite powder particle which loses the spherical shape is reduced, and the number of reflections of light is reduced; and after the sphericity calculation of all the single composite powder particles in the field of view of the micro-scanning photo is finished, starting to calculate the deformation rate of the composite powder particles.
3. The optimization method of the ball-milling powder mixing process of the high-sphericity titanium alloy and ceramic reinforcement composite powder according to claim 1, wherein the ball-milling powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps:
(a) Putting the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement body to be optimized and stainless steel grinding balls into a ball milling tank, wherein the mass of the ceramic reinforcement body particles accounts for 1-7% of that of the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement body to be optimized, when the mass ratio of the ceramic reinforcement body particles is increased, the ball milling speed is increased, the ball milling time is prolonged, the sphericity of the composite powder particles is reduced, and the deformation rate is increased; the mass ratio of the stainless steel grinding balls to the mixed powder is 4-5, the spherical titanium alloy particles are mixed particles with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, and the mass ratio of the corresponding mixed particles is 1-2;
(b) Performing ball milling and powder mixing on the composite powder on a planet ball mill, setting the ball milling time to be 4-10 h, the ball milling rotating speed to be 200-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotating for 60-70 min along the same direction and stopping for 5-10 min; the forward and reverse rotation means forward rotation for 25-35 min, stop for 5-10 min and reverse rotation for 25-35 min;
(c) Under the same ball milling rotation speed and ball milling direction, stopping rotating the planetary ball mill every 1h, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method to obtain a group of sphericity and deformability observation data, continuing performing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, wherein the total ball milling and powder mixing time is 7-10 h, taking out at least 3-6 groups successively for observation, and obtaining sphericity and deformability observation data correspondingly.
4. The optimization method of the ball-milling powder mixing process of the high-sphericity titanium alloy and ceramic reinforcement composite powder according to claim 1, wherein the ball-milling powder mixing process of the titanium alloy and ceramic reinforcement composite powder to be optimized specifically comprises the following steps:
(a) Mixing spherical titanium alloy particles to be optimized and ceramic reinforcement body mixed powder, wherein the mass of the ceramic reinforcement body particles accounts for 1-7% of that of the spherical titanium alloy particles to be optimized and the ceramic reinforcement body mixed powder, and taking stainless steel grinding balls with the diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, wherein the mass ratio of the stainless steel grinding balls to the mixed powder is 4-5: 1, the mass ratio of the corresponding mixed particles is 1-2;
(b) Putting the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and stainless steel grinding balls into a ball milling tank, vacuumizing, introducing argon at the speed of 2-3L/s for 2-3 s when the vacuum degree reaches- (0.1-0.2) MPa, and repeating the process for at least 2-3 times;
(c) Placing a ball milling tank in a vacuum state in a planetary ball mill, setting the rotation speed to be 300-400 rpm, setting the ball milling direction to be one-way, rotating for 1-2 hours each time, staying for 5-10 minutes, ensuring the total rotation time to be 5-10 hours, stopping rotating the planetary ball mill every 1 hour, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method to obtain a group of observed sphericity and deformation data, continuing performing ball milling and powder mixing on the powder in the ball milling tank after 5-10 minutes, setting the total ball milling and powder mixing time to be 7-10 hours, taking out at least 3-6 groups successively for observation, and correspondingly obtaining the sphericity and deformation observation data.
5. The optimization method for the ball-milling powder mixing process of the high-sphericity titanium alloy and ceramic reinforcement composite powder according to claim 1, wherein the specific process of tiling and adhering the composite powder on the conductive adhesive in the first step is as follows: shearing 5 multiplied by 15mm conductive adhesive, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a 5 multiplied by 8mm area on the conductive adhesive, spreading 0.5-1 g of composite powder in the area, blowing off the composite powder which is not adhered to the conductive adhesive by using an ear blowing ball, and blowing for at least 10 times.
6. The optimization method for the ball-milling powder mixing process of the high-sphericity titanium alloy and the ceramic reinforcement composite powder according to claim 1, wherein the statistical software used in the second step is Image J software.
7. The optimization method for the ball-milling powder mixing process of the high sphericity titanium alloy and ceramic reinforcement composite powder according to claim 1, wherein the optimization of the process parameters of the titanium alloy and ceramic reinforcement composite powder is realized by using the ball-milling powder mixing deformation rate ω in the step two and listing the number of deformed single composite powder particles and the deformation rate influence table corresponding to the process parameters of the titanium alloy and ceramic reinforcement composite powder.
8. The method for optimizing the ball-milling powder mixing process of the high-sphericity titanium alloy and the ceramic reinforcement composite powder according to any one of claims 1 to 7, wherein the titanium alloy particles are titanium alloy particles having a spherical morphology, and the ceramic reinforcement particles are non-spherical morphology particles having an adhesive ability.
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