CN115415513B - Titanium alloy and ceramic reinforced phase ball milling powder mixing process optimization method based on uniformity - Google Patents
Titanium alloy and ceramic reinforced phase ball milling powder mixing process optimization method based on uniformity Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 243
- 238000000498 ball milling Methods 0.000 title claims abstract description 145
- 239000000919 ceramic Substances 0.000 title claims abstract description 90
- 229910001069 Ti alloy Inorganic materials 0.000 title claims abstract description 89
- 238000002156 mixing Methods 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 69
- 238000005457 optimization Methods 0.000 title claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 127
- 230000003014 reinforcing effect Effects 0.000 claims abstract description 43
- 239000002245 particle Substances 0.000 claims description 57
- 239000000853 adhesive Substances 0.000 claims description 28
- 230000001070 adhesive effect Effects 0.000 claims description 28
- 230000000007 visual effect Effects 0.000 claims description 17
- 238000000227 grinding Methods 0.000 claims description 13
- 239000010935 stainless steel Substances 0.000 claims description 13
- 229910001220 stainless steel Inorganic materials 0.000 claims description 13
- 238000003892 spreading Methods 0.000 claims description 12
- 238000007664 blowing Methods 0.000 claims description 10
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 230000002787 reinforcement Effects 0.000 claims description 4
- 238000001000 micrograph Methods 0.000 claims 1
- 239000010936 titanium Substances 0.000 abstract description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract description 9
- 229910052719 titanium Inorganic materials 0.000 abstract description 9
- 229910045601 alloy Inorganic materials 0.000 abstract description 3
- 239000000956 alloy Substances 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000005070 sampling Methods 0.000 abstract 1
- 239000011812 mixed powder Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 3
- 238000004451 qualitative analysis Methods 0.000 description 3
- 229910000883 Ti6Al4V Inorganic materials 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 238000009827 uniform distribution Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 108010051489 calin Proteins 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001192 hot extrusion Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000011156 metal matrix composite Substances 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- NMJKIRUDPFBRHW-UHFFFAOYSA-N titanium Chemical compound [Ti].[Ti] NMJKIRUDPFBRHW-UHFFFAOYSA-N 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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Abstract
The invention relates to an optimization method of a titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity, which comprises the steps of sampling composite powder of the ball milling powder mixing process, taking the whole uniformity M and the area uniformity alpha in the ball milling powder mixing process of the titanium alloy and ceramic reinforced phase composite powder, establishing a ball milling powder mixing uniformity model of the titanium alloy and ceramic reinforced phase composite powder, and taking the composite powder ball milling powder mixing uniformity model as a basis, so that the influence of process parameters on the uniformity of the ball milling powder mixing of the composite powder for preparing a reticular titanium-based composite material can be accurately described, thereby optimizing the preparation process parameters of the composite powder of the metal-based composite material, further obtaining uniformly distributed titanium alloy and ceramic reinforced phase composite powder, and facilitating industrial application; meanwhile, the optimization process can be applied to ball milling powder mixing processes of other alloy or ceramic reinforcing 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 demands on the 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 heat resistance and high strength of the ceramic phase, and compared with the traditional titanium alloy, the ceramic reinforcing 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, ceramic reinforcing phase powder and 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 damaging the shapes of the spherical titanium alloy particles, and composite powder of titanium alloy and ceramic reinforcing phase uniformly distributed on the surfaces of the titanium alloy in a net shape can be obtained, and the net-shaped titanium-based composite prepared by the high-quality composite powderThe composite material can obviously improve the plastic workability of the titanium-based composite material, and further improve the room temperature and high temperature mechanical properties of the ceramic reinforced titanium-based composite material. Document 1"Attar H, bonisch M, calin M, et al Selective laser melting of in situ titanium-titanium boridecomposites: processing, microstructure and mechanical properties, acta materials, 2014, 76:13-22," discloses a pure Ti and TiB 2 The ball milling powder mixing method is based on qualitative analysis of composite powder, and preferably selects the ball milling technological parameters of the composite powder. Document 2 "Yang Jianlei. TiB 2 Study on hot extrusion process of Ti-6Al-4V composite powder sheath: the university of Harbin university, shuoshi thesis, 2014 discloses a Ti-6Al-4V and TiB 2 The ball milling powder mixing method adopts a qualitative analysis method to optimize the ball milling process parameters, and the evenly distributed composite powder is obtained. The qualitative analysis method of the composite powder adopted in the above document cannot accurately describe the influence of the ball milling process parameters on the uniformity of the ball milling powder mixture of the composite powder, even if a large amount of ball milling powder mixture test data is still required for specific composite powder, the test result cannot be popularized and applied to the ball milling powder mixture process of other alloy or ceramic reinforcing 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 a method for optimizing the process of ball-milling mixing of titanium alloy and ceramic reinforcing phase based on uniformity of actual process parameters after optimization of ball-milling mixing of composite powder based on quantitative characterization of the uniformity of ball-milling mixing and the influence of process parameters on the uniformity of ball-milling mixing of titanium alloy and ceramic reinforcing phase composite powder.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a method for optimizing a titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity comprises the following steps:
firstly, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking microscopic scanning pictures in the two magnification ranges of 50-80 and 300-400 in each area;
step two, taking a microscopic scanning photo in the 50-80 times range in the step one, and observing whether 10 or more than 10 ceramic reinforcing phase powders are aggregated together in the photo range; the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely the composite powder is determined to be integrally non-uniform, the ceramic reinforcing phase powder in the composite powder is determined to be integrally uniform, and after the integral uniformity determination is completed, the integral uniform 50-80 times of microscopic scanning photos corresponding to 300-400 times of microscopic scanning photos are taken out;
thirdly, taking a microscopic scanning photo of 300-400 times obtained in the second step, and establishing a titanium alloy and ceramic reinforced phase composite powder ball milling powder mixing uniformity model in the view field of the microscopic scanning photo:
in the method, in the process of the invention,
a regional uniformity for the composite powder;S 1 is the sum of areas of free ceramic reinforcing phases, and is expressed in [ mu ] m 2 ；S 2 Is the sum of areas of spherical titanium alloy particles before ball milling and powder mixing, and the unit is [ mu ] m 2 ；n 1 The number of the ceramic reinforcing phases is free;n 2 the number of the spherical titanium alloy particles;ρ 1 the unit is g cm for the density of the ceramic reinforced phase -3 ；ρ 2 Is titanium alloy density in g cm -3 ；ωThe relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areasS 1 Refers to the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photographS T Sum of areas with titanium alloy particlesS J Is the difference between (1);
and step four, optimizing the process parameters of the ball-milling powder mixing of the composite powder according to the calculated uniformity value of the ball-milling powder mixing.
Further, the process for ball milling and mixing the titanium alloy and the ceramic reinforced phase to be optimized specifically comprises the following steps:
(a) Placing spherical titanium alloy particles needing ball milling and powder mixing, ceramic reinforced phase composite powder and stainless steel grinding balls into a ball milling tank, wherein the ceramic reinforced phase accounts for 0.5-8wt% of the composite powder, 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 1:3:6;
(b) Ball milling and mixing the composite powder on a planetary ball mill, wherein the ball milling time is set to be 0.5-10 h, the ball milling rotating speed is set to be 50-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, and the unidirectional rotation means that the composite powder rotates for 60min along the same direction and stops for 5-10 min; the positive and negative rotation means that the rotation is forward for 30min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 30min;
(c) And under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after starting ball milling and mixing powder, opening a ball milling tank to take out 1-2 g of powder, performing the first step, finishing a group of uniformity observation, continuously performing ball milling and mixing on the powder in the ball milling tank after 5-10 min, and sequentially taking out at least 3 groups for uniformity observation.
Further, the specific process of spreading and adhering the composite powder on the conductive adhesive in the first step is as follows: cutting off conductive adhesive with the thickness of 5X (10-15) mm, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a region with the thickness of 5X (5-8) mm on the conductive adhesive, spreading 0.5-1 g of composite powder in the region, blowing off the composite powder which is not adhered on the conductive adhesive by using an ear-blowing ball, and repeatedly blowing at least 5 times.
Further, the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photograph in the step three is obtainedS T The specific steps of (a) are as follows: carrying out color separation processing on the image of the field of view area of the photo according toThe principle that the contrast of titanium alloy particles, ceramic reinforced phase powder and conductive adhesive is different is to mark the free ceramic reinforced phase powder and titanium alloy particles in a visual field area as black, and the area of the black part is automatically calculated to obtain the sum of areasS T In [ mu ] m 2 ；
Further, obtaining the sum of areas of the titanium alloy particles in the field of view of the photograph in the step threeS J The specific steps of (a) are as follows: 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, and automatically calculating the selected area of the red part to obtain the sum of the areas of the titanium alloy particlesS J In [ mu ] m 2 。
Further, the software used for processing the Image of the field of view of the microscope scanning photo is Image pro plus software.
Further, the sum of the areas of the spherical titanium alloy particles before ball milling and powder mixing in the field of view of the photo in the step three is obtainedS 2 ，S 2 In [ mu ] m 2 The following formula is used for calculation:
wherein: s is S J The unit is [ mu ] m of the sum of areas of titanium alloy particles in a microscopic scanning photo field of view 2 The method comprises the steps of carrying out a first treatment on the surface of the R is the average radius of titanium alloy particles, and the unit is mu m; r is the average radius of the ceramic reinforcing phase powder, and the unit is mu m.
Further, the ball milling powder mixing uniformity model is utilized to obtain the region uniformity value of the composite powder
And (3) listing an influence table of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters on the area uniformity of the ball-milling powder mixing composite powder, and realizing optimization of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters.
The beneficial effects of the invention are as follows: titanium alloy and ceramic reinforced phase composite powder ballOverall uniformity M and regional uniformity during milling
The influence of the technological parameters on the uniformity of the ball milling powder mixture for preparing the net-shaped titanium-based composite material can be accurately described based on the defined composite powder ball milling powder mixture uniformity model, so that the preparation technological parameters of the metal-based composite material composite powder are optimized, and the uniformly distributed titanium alloy and ceramic reinforced phase composite powder is obtained, thereby facilitating industrial application; meanwhile, the optimization process can be applied to ball milling powder mixing processes of other alloy or ceramic reinforcing phases.
Drawings
Fig. 1: ti6242 and TiB for defined ball-milled powders 2 A composite powder overall uniformity diagram, wherein (a) is an overall uniformity diagram and (b) is an overall non-uniformity diagram;
fig. 2: ti6242 and TiB for defined ball-milled powders 2 A scanned image photograph of the composite powder overall non-uniformity, wherein (a) is a low-magnification scanned image photograph and (b) is a high-magnification scanned image photograph;
fig. 3: ball milling mixed powder Ti6242/TiB under different ball milling time 2 A high magnification scanned image photograph of the composite powder, wherein (a) is 3h and (b) is 7h;
fig. 4: to quantitatively ball mill mixed powder Ti6242/TiB by adopting Image pro plus software 2 Area S of composite powder J And S is T Schematic of (2);
fig. 5: for ball milling process parameter pair Ti6242/TiB 2 The uniformity of the mixed powder area of the composite powder ball mill is affected.
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: a method for optimizing a titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity comprises the following steps:
firstly, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking microscopic scanning pictures in the two magnification ranges of 50-80 and 300-400 in each area; the specific process of the composite powder being flatly adhered on the conductive adhesive is as follows: cutting off conductive adhesive with the thickness of 5X (10-15) mm, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a region with the thickness of 5X (5-8) mm on the conductive adhesive, spreading 0.5-1 g of composite powder in the region, blowing off the composite powder which is not adhered on the conductive adhesive by using an ear-blowing ball, and repeatedly blowing at least 5 times.
Step two, taking a microscopic scanning photo in the 50-80 times range in the step one, and observing whether 10 or more than 10 ceramic reinforcing phase powders are aggregated together in the photo range; the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely the composite powder is determined to be integrally non-uniform, the ceramic reinforcing phase powder in the composite powder is determined to be integrally uniform, and after the integral uniformity determination is completed, the integral uniform 50-80 times of microscopic scanning photos corresponding to 300-400 times of microscopic scanning photos are taken out;
thirdly, taking a microscopic scanning photo of 300-400 times obtained in the second step, and establishing a titanium alloy and ceramic reinforced phase composite powder ball milling powder mixing uniformity model in the view field of the microscopic scanning photo:
in the method, in the process of the invention,
a regional uniformity for the composite powder;S 1 is the sum of areas of free ceramic reinforcing phases, and is expressed in [ mu ] m 2 ；S 2 Is the sum of areas of spherical titanium alloy particles before ball milling and powder mixing, and the unit is [ mu ] m 2 ；n 1 The number of the ceramic reinforcing phases is free;n 2 the number of the spherical titanium alloy particles;ρ 1 the unit is g cm for the density of the ceramic reinforced phase -3 ；ρ 2 Is titanium alloy density in g cm -3 ；ωThe relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areasS 1 Refers to the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photographS T Sum of areas with titanium alloy particlesS J Is the difference between (1);
obtaining the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photograph in the step threeS T The specific steps of (a) are as follows: the image of the visual field area of the photo is subjected to color separation treatment, the free ceramic reinforced phase powder and the free spherical titanium alloy particles in the visual field area are marked as black according to the principle that the contrast of the titanium alloy spherical particles, the ceramic reinforced phase powder and the conductive adhesive is different, and the selected areas of the black parts are automatically calculated to obtain the sum of the areasS T In [ mu ] m 2 ；
Obtaining the sum of areas of titanium alloy particles in the field of view of the photograph in the step threeS J The specific steps of (a) are as follows: 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, and automatically calculating the selected area of the red part to obtain the sum of the areas of the titanium alloy particlesS J In [ mu ] m 2 。
Obtaining the sum of areas of spherical titanium alloy particles before ball milling and powder mixing in the field of view of the photograph in the step threeS 2 ，S 2 In [ mu ] m 2 The following formula is used for calculation:
wherein: s is S J The unit is [ mu ] m of the sum of areas of titanium alloy particles in a microscopic scanning photo field of view 2 The method comprises the steps of carrying out a first treatment on the surface of the R is titanium alloyAverage radius of the particles is in [ mu ] m; r is the average radius of the ceramic reinforcing phase powder, and the unit is mu m.
The software used for processing the Image of the microscopic scanning photo field of view area is Image pro plus software.
And step four, optimizing the process parameters of the ball-milling powder mixing of the composite powder according to the calculated uniformity value of the ball-milling powder mixing. Obtaining the regional uniformity value of the composite powder by using the ball milling powder mixing uniformity model
And (3) listing an influence table of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters on the area uniformity of the ball-milling powder mixing composite powder, and realizing optimization of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters. />
The process for ball milling and mixing the titanium alloy and the ceramic reinforced phase powder to be optimized specifically comprises the following steps:
(a) Placing spherical titanium alloy particles needing ball milling and powder mixing, ceramic reinforced phase composite powder and stainless steel grinding balls into a ball milling tank, wherein the ceramic reinforced phase accounts for 0.5-8wt% of the composite powder, 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 1:3:6;
(b) Ball milling and mixing the composite powder on a planetary ball mill, wherein the ball milling time is set to be 0.5-10 h, the ball milling rotating speed is set to be 50-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, and the unidirectional rotation means that the composite powder rotates for 60min along the same direction and stops for 5-10 min; the positive and negative rotation means that the rotation is forward for 30min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 30min;
(c) And under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after ball milling and mixing powder for 3-4h, opening a ball milling tank to take out 1-2 g of powder for carrying out the first step, completing a group of uniformity observation, continuing ball milling and mixing powder in the ball milling tank after 5-10 min, and sequentially taking out at least 3 groups for carrying out uniformity observation.
The invention is suitable forThe mixed powder for various titanium alloy particles with spherical morphology and ceramic reinforcement particles with non-spherical morphology and adhesive capability mainly relates to titanium alloy which 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 optimizes the technological parameters of ball milling powder mixing of the ceramic reinforced phase composite powder, and comprises the following specific implementation steps:
(1) 95g of Ti6242 powder and 5g of TiB 2 Placing the powder into a stainless steel ball grinding tank, and placing 500g of stainless steel grinding balls, wherein TiB 2 The stainless steel grinding balls are irregularly shaped, the average grain diameter is 4 mu m, the Ti6242 powder is spherical grains, the average grain diameter is 96 mu m, the diameters of the stainless steel grinding balls are respectively 10mm, 8mm and 5mm, and the added mass is respectively 50g, 150g and 300g.
(2) For Ti6242/TiB on planetary ball mill 2 The composite powder is subjected to ball milling and powder mixing, the ball milling time is 4-10 h, the ball milling rotating speed is 200, 300 and 400rpm, and the ball milling direction is unidirectional rotation and positive and negative rotation. Wherein, unidirectional rotation means rotation along the same direction for 60min, stop for 10min, forward rotation means rotation in forward direction for 30min, stop for 5min, and reverse rotation for 30min.
(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 a ball milling tank to take out 1g of powder, and carrying out Ti6242/TiB after 10min 2 And (5) continuing ball milling of the composite powder.
(4) Cutting off 5X 15mm conductive film, spreading on a TESCAN Vega 2 LMH tungsten filament scanning electron microscope sample stage, selecting 5X 8mm region on conductive film, and mixing 0.5g 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 using a blowing ball 2 The powder is compounded and repeatedly blown for 10 times.
(5) Ti6242/TiB adhered to the conductive adhesive was measured on a TESCAN Vega 2 LMH tungsten filament scanning electron microscope 2 The composite powder randomly selects 3 areas under 70 and 300 magnifications respectivelyA photograph of the scanned image is taken.
(6) Observing Ti6242/TiB of ball-milling mixed powder 2 Scanned image photograph of composite powder, if TiB in composite powder 2 Less than 10 powder aggregates, determined as uniform overall, ti6242/TiB ball milled 2 The overall uniformity of the composite powder is 1, and the regional uniformity of the ball milling mixed powder of the composite powder is quantified; if TiB in composite powder 2 The powder is concentrated by 10 or more than 10, and is determined to be overall non-uniform, and the Ti6242/TiB of ball-milled mixed powder 2 The overall uniformity of the composite powder is 0, and Ti6242/TiB which is not needed to mix ball milling powder is not needed 2 The composite powder area uniformity continues to be quantified, and the composite powder area uniformity is 0. Ti6242/TiB of ball milling mixed powder 2 The results of the calculation of the overall uniformity of the composite powder are shown in table 1.
(7) Statistical scanning of free TiB in a field of view of an Image photograph using Image pro plus software 2 Area of powder and spherical Ti6242 powder. Opening the file in software, clicking New AOI, selecting a view field area, carrying out color separation treatment on an image photo after the selected view field area, and carrying out color separation treatment on the image photo according to Ti6242 particles and TiB 2 The principle that the contrast of the powder and the conductive adhesive is different can lead the free TiB in the visual field area 2 Marking the powder and Ti6242 powder as red, and automatically calculating the selected area of the red part to obtain the sum of the areasS T （µm 2 ). Likewise, opening the image photo of the selected view field area again, clicking a New AOI and a circular selecting tool, selecting Ti6242 powder in the view field area by using the circular selecting tool, then performing color filling treatment on the selected view field area, marking the selected view field area as red, and automatically calculating the selected area of the red part to obtain the sum of areas of the Ti6242 powderS J （µm 2 ). Free TiB 2 Sum of areasS 1 =S T -S J 。
(8) During the ball milling process, tiB free in the gaps is removed 2 The powder and the rest of the powder are adhered to the surfaces of Ti6242 particles, and the surfaces of the Ti6242 particles in the field of view are approximately considered to be adhered with a layer of TiB 2 The powder is not ball-milled and mixed with the spherical Ti6242 particle area, i.e. the sum of the areas of the spherical titanium alloy particlesS 2 The following formula was used for calculation. Wherein the average radius of Ti6242 particlesR48 μm, tiB 2 Average radius of powderrIs 2 mu m;
wherein:S 2 spherical Ti6242 particle area sum (. Mu.m) before ball milling 2 ）；
S J Sum of areas of Ti6242 particles in the field of view (mum 2 ）。
(9) Ti6242/TiB according to ball milling powder mixing 2 Scanning image photograph of composite powder, counting free TiB in visual field 2 The powder area and Ti6242 particle area were calculated for Ti6242/TiB within this field of view using the following formula 2 Composite powder area uniformity
The value of the sum of the values,
wherein:
ti6242/TiB of ball milling powder mixture 2 Composite powder zone uniformity;
S 1 free TiB 2 Sum of areas (mum) 2 ）；
S 2 Spherical Ti6242 particle area sum (. Mu.m) before ball milling 2 ）；
n 1 Free TiB 2 Is the number of (3);
n 2 number of spherical Ti6242 particles.
(10) When the area uniformity is 1, the Ti6242/TiB of the ball milling mixed powder 2 The uniformity of the composite powder area is best, at this time Ti6242/TiB 2 The ball milling and powder mixing process parameters of the composite powder are optimal process parameters, and the evenly distributed Ti6242/TiB can be obtained 2 A composite powder; uniformity when area
At a value of 0, the Ti6242/TiB of the ball-milling mixed powder 2 The composite powder has the worst regional uniformity. Ti6242/TiB of ball milling mixed powder 2 The results of the calculation of the area uniformity of the composite powder are shown in table 2.
TABLE 1 Ti6242/TiB ball milling powder mix 2 Composite powder overall uniformity value
TABLE 2 Ti6242/TiB ball milling powder mix 2 Composite powder area uniformity value
Conclusion: as can be seen from the above table and FIG. 5, the ball milling direction is opposite to Ti6242/TiB of ball milling mixed powder 2 The overall uniformity and the regional uniformity of the composite powder are not obviously influenced, and the ball milling rotating speed and the ball milling time are used for ball milling Ti6242/TiB of mixed powder 2 The overall uniformity and regional uniformity of the composite powder are relatively affected. Under the same ball milling rotating speed, ti6242/TiB after ball milling is carried out along with the extension of ball milling time 2 The composite powder has improved regional uniformity, but when all TiB 2 When the powder is adhered on the surface of the spherical Ti6242 matrix powder, the ball milling time is prolonged for Ti6242/TiB 2 Composite powder zone uniformity effects. Ti6242/TiB with the increase of ball milling rotation speed 2 The composite powder can be uniformly distributed in shorter ball milling time. In the case of a region uniformity of 1, a uniform distribution of Ti6242/TiB can be obtained 2 And (3) compounding powder. Taking into account the sphericity will affect Ti6242/TiB 2 Fluidity of the composite powder, with increasing ball milling time, more Ti6242/TiB 2 The composite powder was deformed, so that the technological parameters of the invention, namely Ti6242/TiB, were 300rpm ball milling speed, 8 hours ball milling time and unidirectional ball milling direction in experimental example 1, in consideration of sphericity and economic effect on the basis of ensuring uniform distribution 2 Optimum ball milling process parameters of the composite powder.
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 (5)
1. The optimization method of the titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity is characterized by comprising the following steps:
firstly, taking composite powder of a titanium alloy and a ceramic reinforcing phase 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 taking microscopic scanning pictures in the two magnification ranges of 50-80 and 300-400 in each area;
step two, taking a microscopic scanning photo in the 50-80 times range in the step one, and observing whether 10 or more than 10 ceramic reinforcing phase powders are aggregated together in the photo range; the ceramic reinforcing phase powder in the composite powder is integrally distributed and aggregated, namely the composite powder is determined to be integrally non-uniform, the ceramic reinforcing phase powder in the composite powder is determined to be integrally uniform, and after the integral uniformity determination is completed, the integral uniform 50-80 times of microscopic scanning photos corresponding to 300-400 times of microscopic scanning photos are taken out;
thirdly, taking a microscopic scanning photo of 300-400 times obtained in the second step, and establishing a titanium alloy and ceramic reinforced phase composite powder ball milling powder mixing uniformity model in the view field of the microscopic scanning photo:
wherein:
a regional uniformity for the composite powder;S 1 is the sum of areas of free ceramic reinforcing phases, and is expressed in [ mu ] m 2 ；S 2 Is the sum of areas of spherical titanium alloy particles before ball milling and powder mixing, and the unit is [ mu ] m 2 ；n 1 The number of the ceramic reinforcing phases is free;n 2 the number of the spherical titanium alloy particles;ρ 1 the unit is g cm for the density of the ceramic reinforced phase -3 ；ρ 2 Is titanium alloy density in g cm -3 ；ωThe relative mass fraction of the ceramic reinforcing phase;
wherein the sum of the free ceramic reinforcing phase areasS 1 Refers to the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photographS T Sum of areas with titanium alloy particlesS J Is the difference between (1);
the sum of areas of free ceramic reinforcing phase powder and titanium alloy particles in the field of view of the photographS T The specific steps of (a) are as follows: the image of the visual field area of the photo is subjected to color separation treatment, the free ceramic reinforced phase powder and titanium alloy particles in the visual field area are marked as black according to the principle that the contrast of titanium alloy particles, ceramic reinforced phase powder and conductive adhesive is different, and the area selected from the black part is automatically calculated to obtain the sum of areasS T In [ mu ] m 2 ；
The sum of the areas of the titanium alloy particles in the field of view of the photographS J The specific steps of (a) are as follows: 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, and automatically calculating the selected area of the red part to obtain the sum of the areas of the titanium alloy particlesS J In [ mu ] m 2 ；
The sum of the areas of the spherical titanium alloy particles in the visual field of the photo before ball milling and powder mixingS 2 ，S 2 In [ mu ] m 2 The following formula is used for calculation:
wherein: s is S J The unit is [ mu ] m of the sum of areas of titanium alloy particles in a microscopic scanning photo field of view 2 The method comprises the steps of carrying out a first treatment on the surface of the R is the average radius of titanium alloy particles, and the unit is mu m; r is the average radius of the ceramic reinforcing phase powder, and the unit is mu m;
and step four, optimizing the process parameters of the ball-milling powder mixing of the composite powder according to the calculated uniformity value of the ball-milling powder mixing.
2. The optimization method of the homogeneity-based titanium alloy and ceramic reinforced phase ball milling powder mixing process according to claim 1, wherein the titanium alloy and ceramic reinforced phase ball milling powder mixing process to be optimized specifically comprises the following steps:
(a) Placing spherical titanium alloy particles needing ball milling and powder mixing, ceramic reinforced phase composite powder and stainless steel grinding balls into a ball milling tank, wherein the ceramic reinforced phase accounts for 0.5-8wt% of the composite powder, 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 10mm, 8mm and 5mm respectively, and the corresponding mass ratio is 1:3:6;
(b) Ball milling and mixing the composite powder on a planetary ball mill, wherein the ball milling time is set to be 0.5-10 h, the ball milling rotating speed is set to be 50-400 rpm, the ball milling direction is unidirectional rotation or positive and negative rotation, and the unidirectional rotation means that the composite powder rotates for 60min along the same direction and stops for 5-10 min; the positive and negative rotation means that the rotation is forward for 30min, the stop is carried out for 5-10 min, and the reverse rotation is carried out for 30min;
(c) And under the same ball milling rotating speed and ball milling direction, stopping rotating the planetary ball mill every 1h after starting ball milling and mixing powder, opening a ball milling tank to take out 1-2 g of powder, performing the first step, finishing a group of uniformity observation, continuously performing ball milling and mixing on the powder in the ball milling tank after 5-10 min, and sequentially taking out at least 3 groups for uniformity observation.
3. The optimization method of the titanium alloy and ceramic reinforced phase ball milling powder mixing process based on uniformity according to claim 1, wherein the specific process of flatly spreading and adhering the composite powder on the conductive adhesive in the first step is as follows: cutting off conductive adhesive with the thickness of 5X (10-15) mm, spreading the conductive adhesive on a scanning electron microscope sample table, selecting a region with the thickness of 5X (5-8) mm on the conductive adhesive, spreading 0.5-1 g of composite powder in the region, blowing off the composite powder which is not adhered on the conductive adhesive by using an ear-blowing ball, and repeatedly blowing at least 5 times.
4. The optimization method of the homogeneity-based titanium alloy and ceramic reinforcement phase ball milling powder mixing process according to any one of claims 1-3, wherein software adopted for processing the Image of the field of view region of the micrograph is Image pro plus software.
5. The optimization method of the homogeneity-based titanium alloy and ceramic reinforcement phase ball milling powder mixing process according to any one of claims 1-3, wherein the region homogeneity value of the composite powder is obtained by using the ball milling powder mixing homogeneity model
And (3) listing an influence table of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters on the area uniformity of the ball-milling powder mixing composite powder, and realizing optimization of the titanium alloy and ceramic reinforced phase ball-milling powder mixing process parameters. />
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