CN115519126B - Optimization method of ball milling powder mixing process of high sphericity titanium alloy and ceramic reinforcement composite powder - Google Patents
Optimization method of ball milling powder mixing process of high sphericity titanium alloy and ceramic reinforcement composite powder Download PDFInfo
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Abstract
The invention relates to an optimization method of a high sphericity titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process, which comprises the steps of taking a composite powder microscopic scanning photo of a titanium alloy and ceramic reinforcement obtained under the process parameters of ball milling powder mixing to be optimized; and calculating the deformation rate omega of the composite powder particles in the view field of the microscopic scanning photo, and finally, taking the process parameters corresponding to the deformation rate lower than 10% as optimized ball milling powder mixing process parameters. According to the method, the sphericity Q and the deformation rate omega of the individual composite powder after ball milling and powder mixing are used as the basis, the process parameters of ball milling and powder mixing of the titanium alloy composite powder are optimized, the optimized process parameters are used for preparing the titanium alloy composite powder with high sphericity, industrial application is facilitated, and manpower and material resources are reduced; meanwhile, the optimization process can be applied to ball milling and powder mixing processes of other alloys or ceramic reinforcements.
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 anti-fatigue, anti-creep and anti-corrosion properties and the like, and is mainly used for manufacturing parts of air compressor components of aeroengines, such as blades, air compressor discs, brakes and the like, and key structural parts of rockets, missiles and high-speed aircrafts; and has a great deal of application in the fields of electrolysis, power stations, petroleum, sea water desalination, environmental pollution control and the like. However, further improvements are needed to meet more demanding service conditions based on their excellent combination of properties. At present, the highest 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 titanium alloy components, the high-temperature mechanical properties and the service temperature of the titanium alloy are required to be further improved. Research shows that the titanium-based composite material prepared by adopting the in-situ self-generation reinforced phase method is one of effective ways for solving the problem.
Since physical properties of the titanium alloy composite powder, such as particle size, sphericity, directly affect the properties of the titanium matrix composite and components, in situ self-generated titanium matrix composite puts stringent demands on the alloy powder. The preparation method of the titanium alloy composite powder refers to a ball milling powder mixing method which enables different alloy powders to be combined uniformly through a physical extrusion method under a certain ball milling condition.
The ball milling mixed powder preparation method adopting the composite powder can provide raw materials for preparing the titanium-based composite material and additive manufacturing of titanium-based composite material components, and is effectively applied to manufacturing 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 compoistes [ J]Acta Materiae Compositae Sinica,2013,30:90-95 "discloses a TiB 2 And a ball milling and powder mixing method of Ti powder, wherein the ball milling rotating speed is 250r/min, and the ball-to-material ratio is 5:1, obtaining TiB under the condition of ball milling time of 11h 2 Ti alloy composite powder.
In the ball milling powder mixing process of the titanium alloy and the reinforcement composite powder, if the composite powder loses the spherical shape, the composite powder becomes flat, and the mechanical properties of the prepared titanium-based composite material or the manufactured titanium-based composite material component can not meet the requirements. Meanwhile, the ball milling powder mixing of the titanium alloy and reinforcement composite powder is carried out under the condition of no protective atmosphere, and the powder possibly reacts with oxygen in the air, so that the titanium alloy and reinforcement composite powder is oxidized, and the mechanical properties of the prepared titanium-based composite material or the manufactured titanium-based composite material component can not meet the requirements.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the high sphericity titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process optimization method based on the condition that ball milling powder mixing accords with the sphericity and deformation rate of powder, so as to obtain the optimized process parameters of the composite powder ball milling powder mixing.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the optimizing process of ball milling and mixing of high sphericity titanium alloy and ceramic reinforcing composite powder includes the following steps:
firstly, taking composite powder of titanium alloy and ceramic reinforcement body obtained under the process parameters of ball milling and powder mixing to be optimized, spreading and adhering the composite powder on conductive adhesive, randomly selecting at least 3 composite powder areas on the conductive adhesive, and respectively taking microscopic scanning pictures of which the sizes are less than 70-100 times in each area;
marking at least one layer of ceramic reinforcement powder particles adhered to the view field of the micro-scanning photo as single composite powder particles, and counting the total number of the single composite powder particles in the micro-scanning photo as N 2 The number of individual composite powder particles losing the spherical shape is denoted as N 1 The single composite powder particle losing the spherical shape refers to a particle with 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 thirdly, taking the technological parameters corresponding to the deformation rate lower than 10% as optimized ball milling powder mixing technological parameters.
Further, the single sphericity Q in the second step is that any single composite powder particle in the view field of the micro-scanning photo is taken, a maximum inscribed circle and a minimum circumscribed circle of the particle are drawn, two strings are taken on the circle, the circle center is the intersection point of the perpendicular bisectors of the two strings, and the radius is any point distance from the circle center to the circumference; calculating a single sphericity Q of the single composite powder particle, the calculation formula of the single sphericity Q being:
wherein: r is (r) 1 A maximum inscribed circle radius of the composite powder in μm; r is (r) 2 The unit is mu m for the minimum circumcircle radius of the composite powder;
when sphericity is 1, the individual composite powder particles are spherical particles of strict meaning; when the sphericity is less than 0.7, the individual composite powder particles are individual composite powder particles losing the spherical shape, the fluidity of the individual composite powder particles losing the spherical shape is reduced, and the number of reflection of light is reduced; after completion of the sphericity calculation of all individual composite powder particles in the field of view of the micrograph, the deformation ratio of the composite powder particles is started to be calculated.
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) Placing the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement needed 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 needed to be optimized, and 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 ratio of the mass of the stainless steel grinding ball to the mass of the mixed powder is (4-5): 1, the spherical titanium alloy particles are mixed particles with diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, and the corresponding ratio of the mass of the mixed particles is (1-2): 3-4): 6-8;
(b) Ball milling and mixing the composite powder on a planetary ball mill, wherein the ball milling time is set to be 4-10 hours, the ball milling rotating speed is 200-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, and the unidirectional rotation means that the composite powder rotates for 60-70 min along the same direction and stops for 5-10 min; the forward rotation and the reverse rotation means that the rotation is forward for 25-35 min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 25-35 min;
(c) Stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening a ball milling tank to take out 1-2 g of powder, performing the optimization method to obtain a group of sphericity and deformation degree observation data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, taking out at least 3-6 groups for observation after the total ball milling and powder mixing time is 7-10 h, and obtaining the sphericity and deformation degree observation data correspondingly.
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 and ceramic reinforcement powder which need to be optimized, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of that of the spherical titanium alloy particles and ceramic reinforcement powder which need to be optimized, and taking stainless steel grinding balls with 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): 3-4): 6-8;
(b) Placing the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and the stainless steel grinding balls into a ball milling tank, vacuumizing, and introducing argon gas for 2-3 s at a rate of 2-3L/s when the vacuum degree reaches- (0.1-0.2) MPa, wherein the process is repeated 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, enabling the ball milling direction to be unidirectional, enabling the ball milling tank to stay for 5-10 min after each rotation for 1-2 h, guaranteeing the total rotation time to be 5-10 h, stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method, obtaining a group of observation sphericity and deformation degree data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, enabling the total ball milling and powder mixing time to be 7-10 h, sequentially taking out at least 3-6 groups for observation, and obtaining sphericity and deformation degree observation data correspondingly.
Further, the specific process of spreading and adhering the composite powder on the conductive adhesive in the first step is as follows: cutting 5X 15mm conducting resin, spreading on a scanning electron microscope sample table, selecting a 5X 8mm area of the conducting resin, spreading 0.5-1 g of composite powder in the area, blowing off the composite powder which is not adhered to the conducting resin by using an ear blowing ball, and blowing for at least 10 times.
Further, the statistical software used in the second step is Image J software.
Further, the deformation rate omega of the ball milling powder mixture in the second step is used for listing the number of deformed single composite powder particles and the deformation rate influence table corresponding to the technological parameters of the powder mixture of the titanium alloy and the ceramic reinforcement, so that the optimization of the technological parameters of the powder mixture of the titanium alloy and the ceramic reinforcement is realized.
Further, 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 beneficial effects of the invention are as follows: according to the method, the sphericity Q and the deformation rate omega of the individual composite powder after ball milling and powder mixing are used as the basis, the process parameters of ball milling and powder mixing of the titanium alloy composite powder are optimized, the optimized process parameters are used for preparing the titanium alloy composite powder with high sphericity, industrial application is facilitated, and manpower and material resources are reduced; meanwhile, the optimization process can be applied to ball milling and powder mixing processes of other alloys or ceramic reinforcements.
Drawings
FIG. 1 is 5wt% TiB 2 An individual powder sphericity quantitative schematic of the Ti6242 alloy composite powder;
FIG. 2 shows the TiB at a rotation speed of 300r/min for a total rotation time of 8h at 5wt% 2 Microstructure photographs of Ti6242 composite powder;
FIG. 3 shows the TiB at a rotation speed of 300r/min at 5wt% for a total rotation time of 9h 2 Microstructure photographs of Ti6242 composite powder;
FIG. 4 shows the TiB at a rotation speed of 300r/min for a total rotation time of 10h at 5wt% 2 Microstructure photographs of Ti6242 composite powder;
FIG. 5 is a graph of 5wt% TiB at a rotational speed of 400r/min for a total rotational time of 5h 2 Microstructure photographs of Ti6242 composite powder;
FIG. 6 is a graph of 5wt% TiB at a rotational speed of 400r/min for a total rotational time of 6h 2 Microstructure photographs of Ti6242 composite powder;
FIG. 7 is a graph of 5wt% TiB at a rotational speed of 400r/min for a total rotational time of 7h 2 Microstructure photograph of Ti6242 composite powder.
Detailed Description
The principles and features of the present invention are described below with reference to the drawings, the examples are illustrated for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
In order to achieve the above object, the present invention provides the following embodiments:
example 1: the optimizing process of ball milling and mixing of high sphericity titanium alloy and ceramic reinforcing composite powder includes the following steps:
firstly, taking composite powder of titanium alloy and ceramic reinforcement body obtained under the process parameters of ball milling and powder mixing to be optimized, spreading and adhering the composite powder on conductive adhesive, randomly selecting at least 3 composite powder areas on the conductive adhesive, and respectively taking microscopic scanning pictures of which the sizes are less than 70-100 times in each area; the specific process of the composite powder flatly adhered on the conductive adhesive is as follows: cutting 5X 15mm conducting resin, spreading on a scanning electron microscope sample table, selecting a 5X 8mm area of the conducting resin, spreading 0.5-1 g of composite powder in the area, blowing off the composite powder which is not adhered to the conducting resin by using an ear blowing ball, and blowing for at least 10 times.
Marking at least one layer of ceramic reinforcement powder particles adhered to the view field of the micro-scanning photo as single composite powder particles, and counting the total number of the single composite powder particles in the micro-scanning photo as N 2 The number of individual composite powder particles losing the spherical shape is denoted as N 1 The single composite powder particle losing the spherical shape refers to a particle with a single sphericity Q of less than 0.7, and the deformation rate ω of the composite powder particle is calculated by the formula:
the single sphericity Q is any single composite powder particle in the view field of the microscopic scanning photo, a maximum inscribed circle and a minimum circumscribed circle of the particle are drawn, two strings are arbitrarily taken on the circle, the circle center is the intersection point of the perpendicular bisectors of the two strings, and the radius is any point distance from the circle center to the circumference; calculating a single sphericity Q of the single composite powder particle, the calculation formula of the single sphericity Q being:
wherein: r is (r) 1 -the maximum inscribed circle radius of the composite powder in μm; r is (r) 2 -the minimum circumcircle radius of the composite powder in μm;
when sphericity is 1, the individual composite powder particles are spherical particles of strict meaning; when the sphericity is less than 0.7, the individual composite powder particles are individual composite powder particles losing the spherical shape, the fluidity of the individual composite powder particles losing the spherical shape is reduced, and the number of reflection of light is reduced; after completion of the sphericity calculation of all individual composite powder particles in the field of view of the micrograph, the deformation ratio of the composite powder particles is started to be calculated.
The statistical software of the deformation rate omega of the composite powder particles is Image J software.
And thirdly, taking the technological parameters corresponding to the deformation rate lower than 10% as optimized ball milling powder mixing technological parameters. And (3) listing the deformation single composite powder particle number and the deformation rate influence table corresponding to the mixing process parameters of the titanium alloy and the ceramic reinforcement by utilizing the ball milling mixing deformation rate omega in the step (II), so as to optimize the mixing process parameters 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:
(a) Placing spherical titanium alloy particles and ceramic reinforcement mixed powder which need 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 spherical titanium alloy particles and ceramic reinforcement mixed powder which need 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 diameters of 10-12 mm, 6-8 mm and 3-5 mm respectively, and the corresponding mass ratio of the mixed particles is (1-2): (3-4): (6-8);
(b) Ball milling and mixing the composite powder on a planetary ball mill, wherein the ball milling time is set to be 4-10 hours, the ball milling rotating speed is 200-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, and the unidirectional rotation means that the composite powder rotates for 60-70 min along the same direction and stops for 5-10 min; the forward rotation and the reverse rotation means that the rotation is forward for 25-35 min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 25-35 min;
(c) Stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening a ball milling tank to take out 1-2 g of powder, performing the optimization method to obtain a group of sphericity and deformation degree observation data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, taking out at least 3-6 groups for observation after the total ball milling and powder mixing time is 7-10 h, and obtaining the sphericity and deformation degree observation data correspondingly.
The titanium alloy particles are titanium alloy particles with spherical morphology, the ceramic reinforcement particles are non-spherical morphology particles with adhesion capability, 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:
(a) Mixing spherical titanium alloy particles and ceramic reinforcement powder which need to be optimized, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of that of the spherical titanium alloy particles and ceramic reinforcement powder which need to be optimized, and taking stainless steel grinding balls with 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): 3-4): 6-8;
(b) Placing the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and the stainless steel grinding balls into a ball milling tank, vacuumizing, and introducing argon gas for 2-3 s at a rate of 2-3L/s when the vacuum degree reaches- (0.1-0.2) MPa, wherein the process is repeated 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, enabling the ball milling direction to be unidirectional, enabling the ball milling tank to stay for 5-10 min after each rotation for 1-2 h, guaranteeing the total rotation time to be 5-10 h, stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method, obtaining a group of observation sphericity and deformation degree data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, enabling the total ball milling and powder mixing time to be 7-10 h, sequentially taking out at least 3-6 groups for observation, and obtaining sphericity and deformation degree observation data correspondingly.
The invention is suitable for mixed powder of titanium alloy particles with spherical morphology and ceramic reinforcement particles with non-spherical morphology, wherein the titanium alloy can be Ti6242 particles or Ti6Al4V particles, and the ceramic reinforcement can be TiB 2 The invention will now be further described by way of experimental examples, either as powder particles or TiC powder particles.
Experimental example 1: as shown in fig. 1-7, the ceramic reinforcement used in this example is TiB 2 Powder particles, titanium alloy particles Ti6242 powder particles, the specific steps of this experimental example are as follows:
(1) Weighing the following components in percentage by mass: tiB of 19 2 Powder particles and Ti6242 powder particles, weighing stainless steel grinding balls with diameters of 5mm, 8mm and 10mm respectively, wherein the mass ratio of the powder to the grinding balls is 1:5, the mass ratio of the grinding balls with different diameters is 6:3:1, a step of;
(2) The weighed Ti6242 powder particles were mixed with 5wt% TiB 2 Placing the powder particles and stainless steel grinding balls into a vacuum grinding tank, vacuumizing, and introducing argon gas for 2s at a rate of 2L/s when the vacuum degree reaches-0.1 MPa, wherein the process is repeated for 3 times;
(3) Placing the vacuum ball milling tank in a planetary ball mill, setting the rotating speed to be 300r/min or 400r/min, wherein the ball milling direction is unidirectional, and the vacuum ball milling tank stays for 10min after each rotation for 1h, and the total rotation time is 5-10 h; stopping rotating the planetary ball mill every 1h, opening a ball milling tank to take out 1-2 g of powder, and performing the optimization method to obtain a group of observation sphericity and deformation degree data, continuously 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, sequentially taking out at least 6 groups for observation, and correspondingly obtaining sphericity and deformation degree observation data;
(4) Observing 6 groups selected in the step 3, and shooting 3 microscopic scanning pictures of different areas under 70 times in each group;
(5) At least one layer of ceramic reinforcement powder particles is drawn adhered in the field of view of the micrograph as a single Ti6242 and 5wt% TiB 2 The method comprises the steps of compounding powder particles, drawing a maximum inscribed circle and a minimum circumscribed circle of single compound powder particles, taking two strings on the circle, wherein the circle center is the intersection point of perpendicular bisectors of the two strings, and the radius is the distance from the circle center to any point of the circumference;
calculation of individual Ti6242 and 5wt% TiB 2 The sphericity Q of the composite powder particles is expressed as:
wherein: Q-Single 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 The minimum circumcircle radius (μm) of the composite powder.
When sphericity is 1, single Ti6242 and 5wt% TiB 2 The composite powder is spherical particles with strict meaning, 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% TiB 2 The composite powder was a composite powder losing the spherical shape, and Ti6242 and 5wt% tib were continuously calculated 2 Deformation rate of the composite powder. After completion of the sphericity calculation of all individual composite powder particles in the field of view of the 6 groups of micrographs, the composite powder particle deformation ratio was started to be calculated.
(6) Ti6242 and 5wt% tib in each photograph were counted using Image J software 2 The total number of composite powders was calculated for all the micrographs for loss of spherical shape Ti6242 and5wt％TiB 2 particle number N of composite powder 1 Ti6242 and TiB with sphericity Q less than 0.7 were counted in each micrograph 2 The amount of composite powder was calculated for Ti6242 and 5wt% TiB in all photographs 2 Total number of particles N2 of the composite powder;
calculation of individual Ti6242 and 5wt% TiB 2 Characterization method of composite powder deformation rate omega. Deformation ratio refers to Ti6242 and 5wt% TiB losing spherical shape 2 Composite powder particle quantity with Ti6242 and 5wt% TiB 2 The percent of the total number of composite powder particles, i.e., the deformation rate ω, is calculated as:
wherein: n (N) 1 Irregular Ti6242 and 5wt% TiB with loss of sphericity in all photographs 2 Number of composite powder particles;
N 2 ti6242 and 5wt% TiB in all photographs 2 Total number of composite powder particles.
When the deformation rate is higher than 10%, ti6242 and 5wt% TiB under the process parameter conditions are indicated 2 The sphericity of the composite powder is low, ti6242 and 5wt% TiB 2 The sphericity of the composite powder does not meet the requirements.
(7) Finally, according to the calculated deformation rate omega, the optimized ball milling powder mixing process parameter is taken as the process parameter corresponding to the deformation rate lower than 10%, thereby realizing the optimization of Ti6242 and 5wt% TiB 2 Ball milling and powder mixing process of composite powder.
Different process parameters to obtain Ti6242 and 5wt% TiB 2 The results of calculating the deformation rate ω of the composite powder are shown in table 1. According to Table 1, ti6242 and 5wt% TiB are preferred 2 The ball milling and powder mixing process parameters of the composite powder are as follows: the ball milling rotating speed is 300r/min, and the total ball milling time is 8h.
TABLE 1 deformation values of Ti6242 and 5wt% TiB2 composite powder
| 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 (individual) | 3088 | 5234 | 3870 | 2380 | 2713 | 2491 |
| Number of deformed particles | 44 | 87 | 78 | 121 | 292 | 402 |
| Deformation ratio (%) | 1.42 | 1.66 | 2.01 | 5.08 | 10.76 | 16.14 |
According to the invention, the ball milling and powder mixing process parameters of the titanium alloy composite powder are optimized based on the sphericity Q and the deformation rate omega of the composite powder after ball milling and powder mixing, and the titanium alloy composite powder with high sphericity is prepared by using the optimized process parameters, so that the industrial application is facilitated, and the manpower and material resources are reduced.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (4)
1. The optimization method of the ball milling powder mixing process of the high sphericity titanium alloy and ceramic reinforcement composite powder is characterized by comprising the following steps:
firstly, taking composite powder of titanium alloy and ceramic reinforcement body obtained under the process parameters of ball milling and powder mixing to be optimized, spreading and adhering the composite powder on conductive adhesive, randomly selecting at least 3 composite powder areas on the conductive adhesive, and respectively taking microscopic scanning pictures of less than 70-100 times in each area;
the specific process of the composite powder being flatly adhered on the conductive adhesive is as follows: cutting conductive adhesive with the thickness of 5 multiplied by 15mm, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a region with the thickness of 5 multiplied by 8mm on the conductive adhesive, spreading 0.5-1 g of composite powder in the region, blowing off the composite powder which is not adhered to the conductive adhesive by using an ear blowing ball, and blowing at least 10 times;
marking the powder particles adhered with at least one layer of ceramic reinforcement in the field of view of the microscopic scanning photo as single composite powder particles, and counting the total number of the single composite powder particles in the microscopic scanning photo as N 2 The number of individual composite powder particles losing the spherical shape is denoted as N 1 The single composite powder particle losing the spherical shape refers to a particle with a single sphericity Q less than 0.7, and the deformation rate omega of the composite powder particle is calculated by a formula:
the single sphericity Q is any single composite powder particle in the view field of the microscopic scanning photo, a maximum inscribed circle and a minimum circumscribed circle of the particle are drawn, two strings are arbitrarily taken on the circle, the circle center is the intersection point of the perpendicular bisectors of the two strings, and the radius is any point distance from the circle center to the circumference; calculating a single sphericity Q of a single composite powder particle, the calculation formula of the single sphericity Q being expressed as:
wherein: r is (r) 1 The maximum inscribed circle radius of the composite powder is in [ mu ] m; r is (r) 2 The minimum circumscribing radius of the composite powder is given in [ mu ] m;
when sphericity is 1, the individual composite powder particles are spherical particles of strict meaning; when the sphericity is less than 0.7, the individual composite powder particles are individual composite powder particles losing the spherical shape, the fluidity of the individual composite powder particles losing the spherical shape is reduced, and the number of reflection of light is reduced; after the sphericity calculation of all single composite powder particles in the field of view of the microscopic scanning photo is completed, the deformation rate of the composite powder particles is calculated;
meanwhile, the deformation rate omega of the ball milling powder mixture is utilized to list the number of deformed single composite powder particles and the deformation rate influence table corresponding to the technological parameters of the titanium alloy and ceramic reinforcement powder mixture, so that the optimization of the technological parameters of the titanium alloy and ceramic reinforcement powder mixture is realized;
step three, taking the technological parameters corresponding to the deformation rate lower than 10% as optimized ball milling powder mixing technological parameters;
the titanium alloy particles of the composite powder of the titanium alloy and the ceramic reinforcement are titanium alloy particles having a spherical morphology, and the ceramic reinforcement particles are non-spherical morphology particles having an adhesive capability.
2. The optimization method of the high sphericity titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process according to claim 1, which is characterized in that the titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process to be optimized specifically comprises the following steps:
(a) Placing spherical titanium alloy particles and ceramic reinforcement mixed powder 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 spherical titanium alloy particles and ceramic reinforcement mixed powder to be optimized, and when the mass ratio of the ceramic reinforcement 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 ratio of the mass of the stainless steel grinding ball to the mass of the mixed powder is 4-5:1, the spherical titanium alloy particles are mixed particles with 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) Ball milling and mixing are carried out on the composite powder on a planetary ball mill, the ball milling time is set to be 4-10 hours, the ball milling rotating speed is 200-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation means that the composite powder rotates for 60-70 min along the same direction, and the composite powder stops for 5-10 min; the forward rotation and the reverse rotation means that the rotation is forward for 25-35 min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 25-35 min;
(c) Stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening a ball milling tank to take out 1-2 g of powder, performing the optimization method to obtain a group of sphericity and deformation degree observation data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, taking out at least 3-6 groups for observation after the total ball milling and powder mixing time is 7-10 h, and obtaining the sphericity and deformation degree observation data correspondingly.
3. The optimization method of the high sphericity titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process according to claim 1, which is characterized in that the titanium alloy and ceramic reinforcement composite powder ball milling powder mixing process to be optimized specifically comprises the following steps:
mixing spherical titanium alloy particles and ceramic reinforcement powder which need to be optimized, wherein the mass of the ceramic reinforcement particles accounts for 1-7% of the mass of the spherical titanium alloy particles and ceramic reinforcement powder which need to be optimized, and taking stainless steel grinding balls with 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, wherein the mass ratio of the corresponding mixed particles is 1-2:3-4:6-8;
placing the mixed powder of the spherical titanium alloy particles and the ceramic reinforcement and the stainless steel grinding balls into a ball milling tank, vacuumizing, and introducing argon gas for 2-3 s at a rate of 2-3L/s when the vacuum degree reaches- (0.1-0.2) MPa, wherein the process is repeated for at least 2-3 times;
placing a ball milling tank in a vacuum state in a planetary ball mill, setting the rotation speed to be 300-400 rpm, enabling the ball milling direction to be unidirectional, enabling the ball milling tank to stay for 5-10 min after each rotation for 1-2 h, guaranteeing the total rotation time to be 5-10 h, stopping rotating the planetary ball mill every 1h under the same ball milling rotation speed and ball milling direction, opening the ball milling tank, taking out 1-2 g of powder, performing the optimization method, obtaining a group of observation sphericity and deformation degree data, continuing ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, enabling the total ball milling and powder mixing time to be 7-10 h, sequentially taking out at least 3-6 groups for observation, and obtaining sphericity and deformation degree observation data correspondingly.
4. The optimization method of the ball milling and powder mixing process of the high sphericity titanium alloy and ceramic reinforcement composite powder according to any one of claims 1 to 3, wherein the statistical software used in the second step is Image J software.
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