CN115415513A - Method for optimizing titanium alloy and ceramic reinforced phase ball-milling powder mixing process based on uniformity - Google Patents
Method for optimizing titanium alloy and ceramic reinforced phase ball-milling powder mixing process based on uniformity Download PDFInfo
- Publication number
- CN115415513A CN115415513A CN202211167991.3A CN202211167991A CN115415513A CN 115415513 A CN115415513 A CN 115415513A CN 202211167991 A CN202211167991 A CN 202211167991A CN 115415513 A CN115415513 A CN 115415513A
- Authority
- CN
- China
- Prior art keywords
- powder
- ball
- titanium alloy
- milling
- uniformity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Powder Metallurgy (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention relates to a method for optimizing a titanium alloy and ceramic reinforcing phase ball-milling powder mixing process based on uniformity, which comprises the steps of sampling and photographing composite powder of the ball-milling powder mixing process, establishing a titanium alloy and ceramic reinforcing phase composite powder ball-milling powder mixing uniformity model step by using the integral uniformity M and the regional uniformity alpha in the process of ball-milling powder mixing of the titanium alloy and ceramic reinforcing phase composite powder, and taking the composite powder ball-milling powder mixing uniformity model as a basis, wherein the influence of process parameters on the ball-milling powder mixing uniformity of the composite powder for preparing a reticular titanium-based composite material can be accurately described, so that the preparation process parameters of the metal-based composite material composite powder are optimized, the uniformly distributed titanium alloy and ceramic reinforcing phase composite powder is obtained, and the industrial application is facilitated; meanwhile, the optimized process can be applied to the ball-milling powder mixing process of other alloy or ceramic reinforced phases.
Description
Technical Field
The invention relates to the field of metal matrix composite materials, in particular to a method for quantitatively optimizing a powder mixing process by adopting ball-milling powder mixing uniformity.
Background
The advanced technology field of aerospace representatives puts higher requirements on high reliability, low energy consumption and functional efficiency of equipment. The main bearing member made of high-performance light metal can meet the requirements of reducing the structural weight of key members of high-end equipment and improving the service performance of the equipment. The titanium-based composite material prepared by compounding the titanium alloy and the ceramic reinforcing phase can simultaneously exert the advantages of high strength and toughness of the titanium alloy and high strength of the ceramic phase, and compared with the traditional titanium alloy, the ceramic reinforced titanium-based composite material has higher strength, modulus, wear resistance, heat resistance, high durability and service temperature, and can be used for a long time in a complex and severe environment.
In the manufacturing process of the titanium-based composite material, the ceramic reinforcing phase powder and the spherical titanium alloy particles are uniformly mixed, so that the ceramic reinforcing phase powder is uniformly distributed on the surfaces of the spherical titanium alloy particles under the condition of not destroying the shapes of the spherical titanium alloy particles, the titanium alloy and the ceramic reinforcing phase composite powder which is uniformly distributed on the surfaces of the titanium alloy in a net shape can be obtained, the plastic processability of the titanium-based composite material can be obviously improved by the net-shaped titanium-based composite material prepared from the high-quality composite powder, and the room-temperature and high-temperature mechanical properties of the ceramic reinforced titanium-based composite material are further improved. Document 1-Attar H, bonisch M, calin M, et al.Selective laser scaling of in situ titanium-titanium compounds Processing, microstructure and mechanical properties. Acta materials, 2014,76 "discloses a pure Ti and TiB material 2 The ball milling powder mixing method is based on the qualitative analysis of the composite powder, and the ball milling technological parameters of the composite powder are optimized. Document 2-Yang Jian Lei. TiB 2 Research on a/Ti-6 Al-4V composite powder sheath hot extrusion process, harbin: the Master academic thesis of Harbin Industrial university, 2014 "discloses a Ti-6Al-4V and TiB 2 The ball milling powder mixing method adopts a method for qualitatively analyzing the uniformity of the composite powder to optimize ball milling process parameters, and the uniformly distributed composite powder is obtained. The qualitative analysis method for composite powder adopted in the above document cannot accurately describe the influence of ball milling process parameters on the ball milling and powder mixing uniformity of the composite powder, and a large number of balls are still needed for specific composite powderThe test data of the powder milling and mixing are provided, and the test result can not be popularized and applied to the powder milling and mixing process of other alloy or ceramic reinforced phases, and the defects of non-optimization, financial consumption, time consumption and the like exist.
Disclosure of Invention
The invention aims to avoid the defects of the prior art and provides an optimization method of a titanium alloy and ceramic reinforced phase ball-milling powder mixing process based on the quantitative characterization of the ball-milling powder mixing uniformity and the influence of process parameters on the ball-milling powder mixing uniformity of the titanium alloy and ceramic reinforced phase composite powder, so that the actual process parameters after the optimization of the ball-milling powder mixing of the composite powder are obtained.
In order to achieve the purpose, the invention adopts the technical scheme that: an optimization method of a titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity comprises the following steps:
step one, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking a micro-scanning picture in each area at two magnification ranges of 50-80 and 300-400 respectively;
step two, taking the micro-scanning picture of the 50-80 times range in the step one, and observing whether the ceramic reinforcing phase powder has a distribution aggregation phenomenon that 10 or more than 10 ceramic reinforcing phase powders are aggregated in the picture range; the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely, the ceramic reinforcing phase powder is determined to be integrally uneven, the ceramic reinforcing phase powder in the composite powder is not distributed and aggregated, namely, the ceramic reinforcing phase powder is determined to be integrally even, and after the integral evenness is determined, the integral even microscopic scanning picture of 300-400 times corresponding to the integral even microscopic scanning picture of 50-80 times is taken out;
step three, taking a microscopic scanning picture of 300-400 times obtained in the step two, and establishing a titanium alloy and ceramic reinforcing phase composite powder ball-milling and powder-mixing uniformity model in a visual field of the microscopic scanning picture:
wherein α is the area uniformity of the composite powder; s 1 Is the sum of the areas of free ceramic reinforcing phases and has the unit of mum 2 ；S 2 Is the sum of the areas of the spherical titanium alloy particles before ball milling and powder mixing, and the unit is mum 2 ；n 1 The number of free ceramic reinforcing phases; n is a radical of an alkyl radical 2 The number of the spherical titanium alloy particles; rho 1 The unit is g cm for ceramic reinforcing phase density -3 ；ρ 2 Is the density of the titanium alloy and has the unit of g cm -3 (ii) a Omega is the relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areas S 1 Refers to the sum S of the areas of free ceramic reinforcing phase powder and titanium alloy particles in a photo field T Sum of area S of titanium alloy particles J A difference of (d);
and step four, optimizing the technological parameters of the ball-milling and powder-mixing of the composite powder according to the calculated uniformity value of the ball-milling and powder-mixing.
Further, the process for ball-milling and mixing the titanium alloy to be optimized and the ceramic reinforcing phase specifically comprises the following steps:
(a) Putting spherical titanium alloy particles, ceramic reinforcing phase composite powder and stainless steel grinding balls which need to be subjected to ball-milling powder mixing into a ball-milling tank, wherein the mass ratio of the ceramic reinforcing phase to the composite powder is 0.5-8 wt%, the mass ratio of the stainless steel grinding balls to the composite powder is (2-7): 1, the diameters of the stainless steel grinding balls are respectively 10mm, 8mm and 5mm, and the corresponding mass ratio is 1;
(b) Performing ball milling and powder mixing on the composite powder on a planetary ball mill, setting the ball milling time to be 0.5-10 h, the ball milling rotation speed to be 50-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotation in the same direction for 60min and stopping for 5-10 min; the forward and reverse rotation means forward rotation for 30min, stop for 5-10 min and reverse rotation for 30min;
(c) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after the ball milling and powder mixing are started, opening the ball milling tank to take out 1-2 g of powder, completing a group of uniformity observation after the first step, continuing to perform ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, and taking out at least 3 groups of powder in sequence for uniformity observation.
Further, the concrete process of laying and adhering the composite powder on the conductive adhesive in the first step is as follows: shearing conductive adhesive with the thickness of 5 multiplied by (10-15) mm, paving the conductive adhesive on a sample table of a scanning electron microscope, selecting a 5 multiplied by (5-8) mm area on the conductive adhesive, paving 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 a blowing lug, and repeatedly blowing for at least 5 times.
Further, the sum S of the areas of the free ceramic reinforcing phase powder and the titanium alloy particles in the photo field in the step three is obtained T The method comprises the following specific steps: carrying out color separation processing on the image of the photo field area, marking free ceramic reinforcing phase powder and titanium alloy particles in the field area as black according to the principle that the contrast of titanium alloy particles, ceramic reinforcing phase powder and conductive adhesive is different, automatically calculating the selected area of the black part to obtain the area sum S T In units of μm 2 ；
Further, the sum S of the areas of the titanium alloy particles in the photo field in the third step is obtained J The method comprises the following specific steps: selecting titanium alloy particles in the visual field area of the photo, then performing color filling treatment on the selected visual field area, marking the selected visual field area as red, automatically calculating the selected area of the red part to obtain the sum S of the areas of the titanium alloy particles J In units of μm 2 。
Furthermore, the software used for processing the Image of the field of view area of the micro-scanning photo is Image pro plus software.
Further, the sum S of the areas of the spherical titanium alloy particles which are not subjected to ball milling and powder mixing in the photo field of view in the step three is obtained 2 ，S 2 Unit is mum 2 The following formula is adopted for calculation:
in the formula: s J Is the sum of the areas of the titanium alloy particles in the field of view of the micro-scanning photograph, and has the unit of mum 2 (ii) a R is the average radius of the titanium alloy particles and has the unit of mu m; r is the average radius of the ceramic reinforcing phase powder in μm.
Further, the ball-milling powder mixing uniformity model is utilized to obtain a zone uniformity value alpha of the composite powder, and the influence table of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters on the zone uniformity of the ball-milling powder mixing composite powder is listed, so that the optimization of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters is realized.
The beneficial effects of the invention are: the influence of process parameters on the ball milling and powder mixing uniformity of the composite powder for preparing the reticular titanium-based composite material can be accurately described by taking the overall uniformity M and the regional uniformity alpha in the ball milling and powder mixing process of the titanium alloy and ceramic reinforcing phase composite powder, namely the defined composite powder ball milling and powder mixing uniformity model as the basis, so that the preparation process parameters of the metal-based composite material composite powder are optimized, the uniformly distributed titanium alloy and ceramic reinforcing phase composite powder is obtained, and the industrial application is facilitated; meanwhile, the optimization process can be applied to the ball-milling powder mixing process of other alloy or ceramic reinforced phases.
Drawings
FIG. 1: ti6242 and TiB being defined ball-milled mixed powders 2 The overall uniformity of the composite powder is shown schematically, wherein (a) is an overall uniformity diagram, and (b) is an overall non-uniformity diagram;
FIG. 2 is a schematic diagram: ti6242 and TiB as defined ball-milled powders 2 Photographs of scanned images of the bulk inhomogeneities of the composite powder, wherein (a) is a photograph of a low-magnification scanned image and (b) is a photograph of a high-magnification scanned image;
FIG. 3: ball-milling mixed powder Ti6242/TiB under different ball-milling time 2 High magnification scanning image photographs of the composite powder, wherein (a) is 3 hours and (b) is 7 hours;
FIG. 4: adopts Image pro plus software to quantitatively ball mill and mix Ti6242/TiB powder 2 Area S of composite powder J And S T A schematic diagram of (a);
FIG. 5 is a schematic view of: is a ball milling process parameter pair Ti6242/TiB 2 Influence of the uniformity of the powder ball milling and mixing area of the 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.
To achieve the above object, the present invention provides the following embodiments:
example 1: an optimization method of a titanium alloy and ceramic reinforced phase ball-milling powder mixing process based on uniformity comprises the following steps:
step one, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking a micro-scanning picture in each area in a range of 50-80 and 300-400 magnification times respectively; the concrete process of the composite powder tiled and adhered on the conductive adhesive comprises the following steps: cutting off 5 x (10-15) mm of conductive adhesive, spreading the conductive adhesive on a sample table of a scanning electron microscope, selecting a 5 x (5-8) mm 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 repeatedly blowing for at least 5 times.
Taking the micro-scanning picture of the 50-80 times range in the step one, and observing whether the ceramic reinforcing phase powder has a distribution aggregation phenomenon that 10 or more than 10 ceramic reinforcing phase powders are aggregated in the picture range; the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely, the ceramic reinforcing phase powder is determined to be integrally uneven, the ceramic reinforcing phase powder in the composite powder is not distributed and aggregated, namely, the ceramic reinforcing phase powder is determined to be integrally even, and after the integral evenness is determined, the integral even microscopic scanning picture of 300-400 times corresponding to the integral even microscopic scanning picture of 50-80 times is taken out;
step three, taking a microscopic scanning picture of 300-400 times obtained in the step two, and establishing a titanium alloy and ceramic reinforcing phase composite powder ball-milling and powder-mixing uniformity model in a visual field of the microscopic scanning picture:
wherein α is the area uniformity of the composite powder; s 1 Is the sum of the areas of free ceramic reinforcing phases and has the unit of mum 2 ；S 2 Is the sum of the areas of the spherical titanium alloy particles before ball milling and powder mixing, and the unit is mum 2 ；n 1 The number of free ceramic reinforcing phases; n is a radical of an alkyl radical 2 The number of the spherical titanium alloy particles; ρ is a unit of a gradient 1 The unit is g cm for ceramic reinforcing phase density -3 ；ρ 2 Is the density of the titanium alloy and has the unit of g cm -3 (ii) a Omega is the relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areas S 1 Refers to the sum S of the areas of free ceramic reinforcing phase powder and titanium alloy particles in a photo field T Sum of area S of titanium alloy particles J A difference of (d);
obtaining the sum S of the areas of the free ceramic reinforcing phase powder and the titanium alloy particles in the photo field in the step three T The method comprises the following specific steps: carrying out color separation processing on the image of the photo field area, marking free ceramic reinforcing phase powder and spherical titanium alloy particles in the field area as black according to the principle that the contrast of the titanium alloy spherical particles and the ceramic reinforcing phase powder with the conductive adhesive is different, automatically calculating the selected area of the black part to obtain the area sum S T In units of μm 2 ；
Obtaining the sum S of the areas of the titanium alloy particles in the visual field of the photo in the third step J The method comprises the following specific steps: selecting titanium alloy particles in the visual field area of the photo, then performing color filling treatment on the selected visual field area, marking the selected visual field area as red, automatically calculating the selected area of the red part to obtain the sum S of the areas of the titanium alloy particles J In units of μm 2 。
Obtaining the photo field of view in the third stepThe sum S of the areas of the spherical titanium alloy particles before the ball milling and the powder mixing 2 ，S 2 Unit is mum 2 The following formula is adopted for calculation:
in the formula: s J Is the sum of the areas of the titanium alloy particles in the field of view of the micro-scanning photograph, and has the unit of mum 2 (ii) a R is the average radius of the titanium alloy particles and has a unit of mu m; r is the average radius of the ceramic reinforcing phase powder in μm.
And the software for processing the Image of the field area of the micro-scanning photo is Image pro plus software.
And step four, optimizing the technological parameters of the ball-milling and powder-mixing of the composite powder according to the calculated uniformity value of the ball-milling and powder-mixing. And obtaining a regional uniformity value alpha of the composite powder by using the ball-milling powder mixing uniformity model, and listing a table of the influence of the technological parameters of the titanium alloy and ceramic reinforced phase ball-milling powder mixing on the regional uniformity of the ball-milling powder mixing composite powder, so that the optimization of the technological parameters of the titanium alloy and ceramic reinforced phase ball-milling powder mixing is realized.
The process for ball-milling and mixing the titanium alloy and the ceramic reinforcing phase to be optimized specifically comprises the following steps:
(a) Putting spherical titanium alloy particles, ceramic reinforcing phase composite powder and stainless steel grinding balls which need to be subjected to ball milling and powder mixing into a ball milling tank, wherein the mass ratio of the ceramic reinforcing phase to the composite powder is 0.5-8 wt%, the mass ratio of the stainless steel grinding balls to the composite powder is (2-7): 1, the diameters of the stainless steel grinding balls are respectively 10mm, 8mm and 5mm, and the corresponding mass ratio is 1;
(b) Performing ball milling and powder mixing on the composite powder on a planet ball mill, setting the ball milling time to be 0.5-10 h, the ball milling rotation speed to be 50-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotation in the same direction for 60min and stopping for 5-10 min; the forward and reverse rotation means forward rotation for 30min, stop for 5-10 min and reverse rotation for 30min;
(c) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after ball milling and mixing for 3-4h, opening the ball milling tank to take out 1-2 g of powder to complete a group of uniformity observation after the first step, continuing ball milling and mixing the powder in the ball milling tank after 5-10 min, and taking out at least 3 groups of powder in sequence to perform uniformity observation.
The invention is suitable for the mixed powder of a plurality of titanium alloy particles with spherical forms and ceramic reinforcement particles with non-spherical forms and adhesive capacity, the mainly related titanium alloy can be any titanium alloy such as Ti6242, TC4 and the like, and the ceramic reinforcement phase can be TiB 2 Powder B 4 Powder C, etc., the present invention will now be further described by way of experimental examples.
Experimental example: as shown in FIGS. 1-5, the present example takes the form of a spherical Ti6242 titanium alloy and TiB 2 The invention relates to ceramic reinforcing phase composite powder, which optimizes the technological parameters of ball milling and mixing the ceramic reinforcing phase composite powder and comprises the following specific implementation steps:
(1) 95g of Ti6242 powder and 5g of TiB 2 Putting the powder into a stainless steel ball milling tank, and then putting 500g of stainless steel grinding balls, wherein the powder is TiB 2 The powder was irregular in shape and had an average particle size of 4 μm, the Ti6242 powder was spherical in shape and had an average particle size of 96 μm, the stainless steel grinding balls had diameters of 10mm, 8mm and 5mm, respectively, and the masses added were 50g, 150g and 300g, respectively.
(2) On a planetary ball mill to Ti6242/TiB 2 And ball milling and mixing the composite powder for 4-10 h at the ball milling rotation speed of 200, 300 and 400rpm in one-way rotation and positive and negative rotation directions. Wherein, the unidirectional rotation means rotating for 60min and stopping for 10min along the same direction, and the positive and negative rotation means rotating for 30min in the forward direction, stopping for 5min and rotating for 30min in the reverse direction.
(3) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after ball milling for 4h, opening the ball milling tank to take out 1g of powder, and performing ball milling on Ti6242/TiB after 10min 2 And continuously ball-milling the composite powder.
(4) Cutting 5 × 15mm conductive adhesive, spreading on TESCAN Vega 2LMH tungsten filament scanning electron microscope sample stage, selecting 5 × 8mm region on the conductive adhesiveDomain, 0.5g of Ti6242/TiB 2 The composite powder is spread in the area, and Ti6242/TiB which is not adhered to the conductive adhesive is blown off by an ear blowing ball 2 The powder was compounded and blown repeatedly 10 times.
(5) On a scanning electron microscope with a TESCAN Vega 2LMH tungsten filament, ti6242/TiB adhered on a conductive adhesive is added 2 The composite powder was photographed in scanned images by randomly selecting 3 regions at 70 and 300 magnifications, respectively.
(6) Ti6242/TiB for observing ball-milling mixed powder 2 Scanning image of composite powder, if TiB in composite powder 2 Less than 10 powder aggregates, determined as homogeneous whole, ball-milled powder of Ti6242/TiB 2 Quantifying the regional uniformity of the ball-milling mixed powder of the composite powder if the overall uniformity of the composite powder is 1; if TiB in the composite powder 2 The powder is gathered by 10 and more than 10 and determined as the Ti6242/TiB which is not uniform as a whole and is ball-milled and mixed 2 The integral uniformity of the composite powder is 0, and the Ti6242/TiB of ball-milling mixed powder is not needed 2 If the composite powder area uniformity continues to be quantified, the composite powder area uniformity is 0. Ti6242/TiB of ball-milled mixed powder 2 The results of the calculation of the overall uniformity of the composite powder are shown in table 1.
(7) Image pro plus software is adopted to count TiB dissociating in a certain visual field of a scanned Image photo 2 Area of powder and spherical Ti6242 powder. Opening the file in software, clicking New AOI, selecting a field of view region, performing color separation processing on an image photo after the field of view region is selected, and performing particle and TiB processing according to Ti6242 2 The principle that the contrast of the powder and the conductive adhesive is different can lead free TiB in the field area 2 Marking the powder and the Ti6242 powder as red, automatically calculating the selected area of the red part to obtain the sum S of the areas T (μm 2 ). Similarly, opening the image photo of the selected field area again, clicking a New AOI and a circular selection tool, selecting Ti6242 powder in the field area by using the circular selection tool, then performing color filling processing on the selected field area, marking the selected field area as red, automatically calculating the selected area of the red part to obtain the sum S of the areas of the Ti6242 powder J (μm 2 ). Free TiB 2 Sum of area S 1 ＝S T -S J 。
(8) In the ball milling process, the TiB dissociated in the clearance is removed 2 The powder, the rest of the powder adhered to the surface of the Ti6242 particle, and the surface of the Ti6242 particle in the field of view was considered to be adhered with a layer of TiB 2 The area of the spherical Ti6242 particles before ball milling and mixing is the sum S of the areas of the spherical titanium alloy particles 2 The following formula was used for calculation. Wherein the average radius R of Ti6242 particles is 48 μm, tiB 2 The average radius r of the powder was 2 μm.
S 2 ＝0.9216×S J
In the formula: s 2 Sum of the areas of spherical Ti6242 particles before ball-milling and mixing (mum) 2 )；
S J Sum of areas of Ti6242 particles in the field of view (. Mu.m) 2 )；
(9) Ti6242/TiB based on ball-milled mixed powder 2 Scanning image photograph of composite powder, counting free TiB in field of view 2 The powder area and the Ti6242 particle area were calculated from Ti6242/TiB in this field of view by the following formula 2 Composite powder area uniformity alpha value.
In the formula: ti6242/TiB of alpha-ball milling mixed powder 2 Composite powder area uniformity;
S 1 free TiB 2 Sum of area (. Mu.m) 2 )；
S 2 Sum of areas of spherical Ti6242 particles before ball-milling and mixing (mum) 2 )；
n 1 Free TiB 2 The number of (2);
n 2 -number of spherical Ti6242 particles.
(10) When the zone uniformity is 1, the Ti6242/TiB of the ball-milled mixed powder 2 The composite powder has the best regional uniformity, and the Ti6242/TiB is adopted 2 Ball milling and powder mixing process of composite powderThe parameters are optimal process parameters, and uniformly distributed Ti6242/TiB can be obtained 2 Compounding powder; when the area uniformity alpha value is 0, the Ti6242/TiB of the ball-milling mixed powder 2 The composite powder region had the worst uniformity. Ti6242/TiB of ball-milling mixed powder 2 The results of the composite powder region uniformity calculations are shown in table 2.
TABLE 1 Ti6242/TiB of ball-milled mixed powders 2 Composite powder bulk uniformity value
| Time of ball milling | 4h | 5h | 6h | 7h | 8h | 9h | 10h |
| 200rpm, one way | 0 | 0 | 0 | 1 | 1 | 1 | 1 |
| 200rpm, front and back | 0 | 0 | 0 | 0 | 0 | 1 | 1 |
| 300rpm, one |
1 | 1 | 1 | 1 | 1 | 1 | 1 |
| 300rpm, forward and reverse | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| 400rpm, one |
1 | 1 | 1 | 1 | 1 | 1 | 1 |
TABLE 2 Ti6242/TiB of ball-milled mixed powders 2 Composite powder area uniformity value
And (4) conclusion: as can be seen from the above table and FIG. 5, the ball milling direction is opposite to the Ti6242/TiB of the ball-milled mixed powder 2 The integral uniformity and the regional uniformity of the composite powder have no obvious influence, and the ball milling rotating speed and the ball milling time have no obvious influence on the Ti6242/TiB of the ball milling mixed powder 2 The influence of the overall uniformity and the regional uniformity of the composite powder is large. Under the same ball milling rotating speed, with the prolonging of the ball milling time, the ball milled Ti6242/TiB 2 The composite powder has improved area uniformity, but when all TiB is 2 When the powder is adhered to the surface of the spherical Ti6242 base powder, the ball milling time is prolonged for Ti6242/TiB 2 Composite powder area uniformity effects. With the increase of the rotation speed of the ball mill, ti6242/TiB 2 The composite powder can be uniformly distributed in a shorter ball milling time. When the regional uniformity reaches 1, the Ti6242/TiB with uniform distribution can be obtained 2 And (3) compounding the powder. Considering that the sphericity affects Ti6242/TiB 2 The fluidity of the composite powder is increased with the increase of the ball milling time, and more Ti6242/TiB 2 The composite powder is deformed, so that on the basis of ensuring uniform distribution, the process parameters that the ball milling rotating speed is 300rpm, the ball milling time is 8 hours and the ball milling direction is unidirectional in the experimental example 1 are Ti6242/TiB of the invention in consideration of the sphericity and the economic effect 2 And (4) optimal ball milling technological parameters of the composite powder.
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. An optimization method of a titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity is characterized by comprising the following steps:
step one, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking a micro-scanning picture in each area at two magnification ranges of 50-80 and 300-400 respectively;
step two, taking the micro-scanning picture of the 50-80 times range in the step one, and observing whether the ceramic reinforcing phase powder has a distribution aggregation phenomenon that 10 or more than 10 ceramic reinforcing phase powders are aggregated in the picture range; the method comprises the following steps of (1) determining that the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely determining that the composite powder is integrally non-uniform, determining that the ceramic reinforcing phase powder in the composite powder is not distributed and aggregated, namely determining that the composite powder is integrally uniform, and taking out a 300-400 times of micro-scanning picture corresponding to a 50-80 times of micro-scanning picture of the integral uniformity after the integral uniformity is determined;
step three, taking a microscopic scanning picture of 300-400 times obtained in the step two, and establishing a titanium alloy and ceramic reinforcing phase composite powder ball-milling and powder-mixing uniformity model in a visual field of the microscopic scanning picture:
in the formula: α is the area uniformity of the composite powder; s 1 Is the sum of the areas of free ceramic reinforcing phases and has the unit of mum 2 ；S 2 Is the sum of the areas of the spherical titanium alloy particles before ball milling and powder mixing, and the unit is mum 2 ；n 1 The number of free ceramic reinforcing phases; n is 2 The number of the spherical titanium alloy particles; rho 1 The unit is g cm for ceramic reinforcing phase density -3 ；ρ 2 Is the density of the titanium alloy and has the unit of g cm -3 (ii) a Omega is the relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areas S 1 Refers to the sum S of the areas of free ceramic reinforcing phase powder and titanium alloy particles in a photo field T Sum of area S of titanium alloy particles J A difference of (d);
and step four, optimizing the technological parameters of the ball-milling and powder-mixing of the composite powder according to the calculated uniformity value of the ball-milling and powder-mixing.
2. The optimization method of the ball-milling powder mixing process of the titanium alloy and the ceramic reinforcing phase based on the uniformity as claimed in claim 1, wherein the ball-milling powder mixing process of the titanium alloy and the ceramic reinforcing phase to be optimized specifically comprises the following steps:
(a) Putting spherical titanium alloy particles, ceramic reinforcing phase composite powder and stainless steel grinding balls which need to be subjected to ball-milling powder mixing into a ball-milling tank, wherein the mass ratio of the ceramic reinforcing phase to the composite powder is 0.5-8 wt%, the mass ratio of the stainless steel grinding balls to the composite powder is (2-7);
(b) Performing ball milling and powder mixing on the composite powder on a planetary ball mill, setting the ball milling time to be 0.5-10 h, the ball milling rotation speed to be 50-400 rpm, and the ball milling direction to be unidirectional rotation or positive and negative rotation, wherein the unidirectional rotation refers to rotation in the same direction for 60min and stopping for 5-10 min; the forward and reverse rotation means forward rotation for 30min, stop for 5-10 min and reverse rotation for 30min;
(c) Under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after the ball milling and powder mixing are started, opening the ball milling tank to take out 1-2 g of powder, completing a group of uniformity observation after the first step, continuing to perform ball milling and powder mixing on the powder in the ball milling tank after 5-10 min, and taking out at least 3 groups of powder in sequence for uniformity observation.
3. The optimization method of ball milling powder mixing process based on homogeneity of titanium alloy and ceramic reinforcing phase according to claim 1, wherein the specific process of spreading and adhering the composite powder on the conductive adhesive in the first step is as follows: cutting off 5 x (10-15) mm of conductive adhesive, spreading the conductive adhesive on a sample table of a scanning electron microscope, selecting a 5 x (5-8) mm 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 repeatedly blowing for at least 5 times.
4. The optimization method for the homogeneity-based ball-milling powder mixing process of titanium alloy and ceramic reinforcing phase according to claim 1, wherein the sum S of the areas of the free ceramic reinforcing phase powder and the titanium alloy particles in the photo field in the third step is obtained T The method comprises the following specific steps: carrying out color separation processing on the image of the photo field area, marking free ceramic reinforcing phase powder and titanium alloy particles in the field area as black according to the principle that the contrast of the titanium alloy particles, the ceramic reinforcing phase powder and the conductive adhesive is different, selecting areas of the black parts for automatic calculation to obtain the sum S of the areas T In units of μm 2 。
5. The optimization method for the ball milling powder mixing process of titanium alloy and ceramic reinforcing phase based on uniformity as claimed in claim 1, wherein the sum S of the areas of the titanium alloy particles in the photo field of view in the third step is obtained J The method comprises the following specific steps: selecting titanium alloy particles in the field of view of the photo, performing color filling treatment on the selected field of view, marking the selected field of view as red, and automatically calculating the selected area of the red part to obtain the sum S of the areas of the titanium alloy particles J In units of μm 2 。
6. The optimization method for the homogeneity-based ball-milling powder-mixing process of titanium alloy and ceramic-reinforced phase according to claim 4 or 5, wherein the software for processing the Image of the field of view area of the micro-scanning photograph is Image pro plus software.
7. The optimization method of ball-milling powder mixing process of titanium alloy and ceramic reinforcing phase based on homogeneity as claimed in claim 1, wherein the sum S of the areas of the spherical titanium alloy particles before ball-milling powder mixing in the photo field of view in the third step is obtained 2 ，S 2 Unit is mum 2 The following formula is adopted for calculation:
in the formula: s J Is the sum of the areas of the titanium alloy particles in the field of view of the micro-scanning photograph, and has the unit of mum 2 (ii) a R is the average radius of the titanium alloy particles and has the unit of mu m; r is the average radius of the ceramic reinforcing phase powder in μm.
8. The optimization method of the titanium alloy and ceramic enhanced phase ball-milling powder mixing process based on the uniformity as claimed in any one of claims 1 to 5 and 7, wherein the ball-milling powder mixing uniformity model is utilized to obtain the regional uniformity value α of the composite powder, and the influence table of the titanium alloy and ceramic enhanced phase ball-milling powder mixing process parameters on the regional uniformity of the ball-milling powder mixing composite powder is listed, so that the optimization of the titanium alloy and ceramic enhanced phase ball-milling powder mixing process parameters is realized.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211167991.3A CN115415513B (en) | 2022-09-23 | 2022-09-23 | Titanium alloy and ceramic reinforced phase ball milling powder mixing process optimization method based on uniformity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211167991.3A CN115415513B (en) | 2022-09-23 | 2022-09-23 | Titanium alloy and ceramic reinforced phase ball milling powder mixing process optimization method based on uniformity |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN115415513A true CN115415513A (en) | 2022-12-02 |
| CN115415513B CN115415513B (en) | 2023-04-28 |
Family
ID=84203594
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211167991.3A Active CN115415513B (en) | 2022-09-23 | 2022-09-23 | Titanium alloy and ceramic reinforced phase ball milling powder mixing process optimization method based on uniformity |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115415513B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101890590A (en) * | 2010-07-01 | 2010-11-24 | 哈尔滨工业大学 | Composite soldering material for soldering titanium alloy and ceramic or ceramic matrix composition material and method for soldering by using same |
| US20130071283A1 (en) * | 2010-05-31 | 2013-03-21 | Toho Titanium Co., Ltd. | Titanium alloy complex powder containing ceramic and process for production thereof, consolidated titanium alloy material using this powder and process for production thereof |
| CN107130138A (en) * | 2017-05-19 | 2017-09-05 | 淮阴工学院 | The method of medical high abrasion titanium alloy composite material and 3D printing gradient in-situ nano complex phase anti-attrition medical titanium alloy |
| CN112030037A (en) * | 2020-08-07 | 2020-12-04 | 南京航空航天大学 | Wear-resistant gradient interface complex-phase reinforced titanium alloy material and preparation method thereof |
| CN113215441A (en) * | 2021-04-21 | 2021-08-06 | 上海材料研究所 | SLM (Selective laser melting) -molding-based nanoparticle reinforced titanium-based composite material and preparation method thereof |
| CN114713832A (en) * | 2022-04-26 | 2022-07-08 | 哈尔滨工业大学 | High-hardness wear-resistant spherical titanium-based composite powder and preparation method thereof |
-
2022
- 2022-09-23 CN CN202211167991.3A patent/CN115415513B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130071283A1 (en) * | 2010-05-31 | 2013-03-21 | Toho Titanium Co., Ltd. | Titanium alloy complex powder containing ceramic and process for production thereof, consolidated titanium alloy material using this powder and process for production thereof |
| CN101890590A (en) * | 2010-07-01 | 2010-11-24 | 哈尔滨工业大学 | Composite soldering material for soldering titanium alloy and ceramic or ceramic matrix composition material and method for soldering by using same |
| CN107130138A (en) * | 2017-05-19 | 2017-09-05 | 淮阴工学院 | The method of medical high abrasion titanium alloy composite material and 3D printing gradient in-situ nano complex phase anti-attrition medical titanium alloy |
| CN112030037A (en) * | 2020-08-07 | 2020-12-04 | 南京航空航天大学 | Wear-resistant gradient interface complex-phase reinforced titanium alloy material and preparation method thereof |
| CN113215441A (en) * | 2021-04-21 | 2021-08-06 | 上海材料研究所 | SLM (Selective laser melting) -molding-based nanoparticle reinforced titanium-based composite material and preparation method thereof |
| CN114713832A (en) * | 2022-04-26 | 2022-07-08 | 哈尔滨工业大学 | High-hardness wear-resistant spherical titanium-based composite powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN115415513B (en) | 2023-04-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105803271B (en) | A kind of aluminum-base nano composite material based on SLM shapings and preparation method thereof | |
| Marks | Surface structure and energetics of multiply twinned particles | |
| Gurao et al. | On the evolution of heterogeneous microstructure and microtexture in impacted aluminum–lithium alloy | |
| CN104946920B (en) | Preparation method of grain refiner | |
| Zhu et al. | Effects of bubbles on high-temperature corrosion of helium ion-irradiated Ni-based alloy in fluoride molten salt | |
| CN115415513A (en) | Method for optimizing titanium alloy and ceramic reinforced phase ball-milling powder mixing process based on uniformity | |
| Zhao et al. | Microstructure evolution and grain refinement mechanism of fine-grained Mg-Gd-Y-Zn-Zr alloy during multi-directional forging | |
| CN111139467A (en) | Laser repair layer containing rare earth oxide on titanium alloy surface and preparation method thereof | |
| Nyberg et al. | The Influence of Casting Conditions on the Microstructure of As-Cast U-10Mo Alloys: Characterization of the Casting Process Baseline | |
| CN1793047A (en) | Process for preparing nuclear shell type composite ceramic particle | |
| He et al. | In-situ investigation on the microstructure evolution of Mg-2Gd alloys during the V-bending tests | |
| Li et al. | Fabrication of particle-reinforced aluminum alloy composite: role of casting and rolling | |
| Chen et al. | Effects of Sn grain size on intermetallic compounds formation in 5 µm diameter Cu/Sn pillar bumps | |
| Kumar et al. | Influence of extrusion process on mechanical and tribological properties of aluminium A356-Al2O3 stir cast MMC | |
| CN115519126B (en) | Optimization method of ball milling powder mixing process of high sphericity titanium alloy and ceramic reinforcement composite powder | |
| Shi et al. | Toughening mechanisms and microstructure of Al2O3–TiC–Co composites | |
| Zhao et al. | 3D characterization of the primary Al3Sc phases in an Al-Sc alloy using Synchrotron X-ray tomography and electron microscopy | |
| Abe | Atomic-scale characterization of nanostructured metallic materials by HAADF/Z-contrast STEM | |
| CN114622147B (en) | Preparation method of array type particle reinforced composite material | |
| Bhavan et al. | EBSD characterization of graphene nano sheet reinforced Sn–Ag solder alloy composites | |
| Sun et al. | Microstructure and Mechanical Properties of TC4 Titanium Alloy by Electron Beam Freeform Fabrication | |
| Hira et al. | Optimizing Gas Injection Stir Casting Process Parameters for Improving the Ultimate Tensile Strength of Hybrid Mg/(SiC Taguchi p Technique | |
| Yao et al. | In-situ evidence for rotation of Si particles with respect to grains in tensile-deformed Al− Si alloys | |
| Madejski et al. | Microstructural and mechanical properties of selective laser melted Inconel 718 for different specimen sizes | |
| Hunn et al. | Fabrication and Characterization of Sixteen SiC Variants Deposited on the Same IPyC Substrate for Fracture Strength Testing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |