CN108555282B - Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof - Google Patents
Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof Download PDFInfo
- Publication number
- CN108555282B CN108555282B CN201810581794.3A CN201810581794A CN108555282B CN 108555282 B CN108555282 B CN 108555282B CN 201810581794 A CN201810581794 A CN 201810581794A CN 108555282 B CN108555282 B CN 108555282B
- Authority
- CN
- China
- Prior art keywords
- aluminum
- titanium
- alloy powder
- powder
- ball milling
- 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.)
- Expired - Fee Related
Links
- 239000000843 powder Substances 0.000 title claims abstract description 63
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 50
- 239000000956 alloy Substances 0.000 title claims abstract description 50
- 230000000694 effects Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000000498 ball milling Methods 0.000 claims abstract description 35
- 239000002245 particle Substances 0.000 claims abstract description 35
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 21
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 15
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 15
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000008117 stearic acid Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000010935 stainless steel Substances 0.000 claims description 23
- 229910001220 stainless steel Inorganic materials 0.000 claims description 23
- 238000001816 cooling Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 238000012856 packing Methods 0.000 abstract description 16
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 229910001069 Ti alloy Inorganic materials 0.000 abstract description 9
- 239000012798 spherical particle Substances 0.000 abstract description 3
- 238000009826 distribution Methods 0.000 description 12
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052782 aluminium Inorganic materials 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 7
- 239000002184 metal Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 239000003814 drug Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 6
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 238000002156 mixing Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000005563 spheronization Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 239000002360 explosive Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000008177 pharmaceutical agent Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005056 compaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005551 mechanical alloying Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002076 thermal analysis method Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
-
- 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
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 discloses a spherical high-activity aluminum-titanium mechanical alloy powder and a preparation method thereof, wherein 62-65% of aluminum powder, 26-28% of titanium powder and 7-11% of stearic acid by weight percentage are added into a ball mill together with a grinding ball and stirred uniformly; starting the ball mill, enabling the ball mill to rotate forwards for 1 minute and then rotate backwards for 1 minute, and then rotate forwards for 1 minute and then rotate backwards for 1 minute, wherein the rotation is used as a ball milling cycle, and then a plurality of ball milling cycles are carried out; and (4) unloading the ball milling tank after ball milling is finished, introducing air for 15 minutes, standing for 24 hours, and taking the material to obtain the spherical high-activity aluminum-titanium mechanical alloy powder. The micro-morphology of the aluminum-titanium alloy powder prepared by the invention is spherical particles, the particle size is very small, and the average particle size d50Less than 8.05 μm, minimum mean particle size d50Reaching 6.22 mu m; the prepared aluminum-titanium alloy powder has very high activity, the thermal reaction temperature does not exceed 845 ℃, and the lowest thermal reaction temperature reaches 565 ℃; the prepared aluminum-titanium alloy powder has very high packing density which is not less than 2.89g/cm3(92% theoretical density), the maximum packing density can reach 3.03g/cm3(94% theoretical density).
Description
Technical Field
The invention relates to the technical field of energetic materials, in particular to spherical high-activity aluminum-titanium mechanical alloy powder and a preparation method thereof.
Background
Among energetic materials, aluminum powder is a high heat additive. The aluminum powder can emit a large amount of heat in the combustion process, so that the combustion temperature of the medicament system is greatly improved. However, as a fuel in energetic materials, aluminum powder has a significant drawback of high ignition temperature, up to 2000 ℃. Such high ignition temperatures limit its use in some specific energetic materials. For example, for some agents, both a sufficient exotherm and a low ignition temperature are required, while a sufficiently high exotherm rate is required. The application of the common aluminum powder can meet the requirement of heat release, but cannot meet the requirements of low ignition temperature and high heat release rate. At this time, the aluminum powder needs to be subjected to ultrafine treatment to meet the requirements. Aluminum is a metal, and the most suitable method for ultrafining it is a mechanical ball milling method. However, aluminum has high ductility, and only flaking of aluminum particles can be achieved during mechanical ball milling, which reduces the specific surface area and does not achieve the purpose of reducing the particle size of aluminum powder. Further, the flaky aluminum powder is not favorable for granulation and molding of the pharmaceutical agent, resulting in a significant decrease in the packing density of the pharmaceutical agent. Researches show that the brittleness of aluminum can be improved and the refinement of aluminum powder can be realized by adding other metals and aluminum to form alloy powder in the ball milling process.
The metal titanium powder is an important component in energetic materials and has very high activity. Titanium powder exposed to air presents a fire hazard. Titanium powder can emit a large amount of heat when burning, can emit hydrogen when reacting with moisture in the air, and has a risk of ignition or explosion when being mixed with an oxidant. The fine titanium powder has strong reducibility, can explode when contacting with hot air and can generate CO2Burning in gas, pure N at over 1000 deg.C2And (4) medium combustion. The explosion occurs when titanium and its alloy powders are treated with nitric acid. In addition, the oil-stained titanium sheet may also be pyrophoric. Titanium powder is often used as an ignition charge for a combustion bomb in military. Therefore, if a small amount of titanium powder and aluminum powder are selected and ball-milled, the aluminum powder can be pulverized. The reduction of the granularity and the treatment of mechanical alloying not only can greatly reduce the ignition temperature of the aluminum powder, but also can ensure high heat release.
The problem of controlling the micro-morphology of the product is also involved in the preparation process of the mechanical alloy powder. The spherical micro-morphology will aid in the mixing of the agents and allow for maximum packing density. The higher the degree of spheronization, the higher the packing density. In addition, controlling the aluminum alloy powder particle size to 10 μm or less greatly reduces the thermal reaction temperature of the aluminum powder, significantly improving the reactivity of the aluminum powder. At present, alloy powder prepared by a common mechanical method is irregular granular particles and flaky substances, the average particle size is usually larger than 20 mu m, and the particle size distribution is wider; in particular, the particle size of the starting powdery aluminum is generally large, the particle size distribution is also broad, and sometimes even a plurality of particle size distribution peaks appear. These will seriously affect the mixing uniformity and packing density of the medicament.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides spherical high-activity aluminum-titanium mechanical alloy powder and a preparation method thereof.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
a spherical high-activity aluminum-titanium mechanical alloy powder is prepared by ball milling the following raw materials in percentage by mass: 62-65% of aluminum powder, 26-28% of titanium powder and 7-11% of stearic acid, wherein the average particle size d of the spherical high-activity aluminum-titanium mechanical alloy powder50Less than 10 μm.
In addition, the invention also provides a preparation method of the spherical high-activity aluminum-titanium mechanical alloy powder, which comprises the following steps:
taking aluminum powder, titanium powder and stearic acid, adding the aluminum powder, the titanium powder and the stearic acid and grinding balls into a ball mill, wherein the mass ratio of the grinding balls to materials is 34-38: 1, uniformly stirring, and the ball mill adopts a YXQM-1L planetary ball mill produced by powder metallurgy research institute of Changshan, Zhongnan university;
starting the ball mill, enabling the ball mill to rotate forwards for 1 minute and then rotate backwards for 1 minute, and then rotate forwards for 1 minute and then rotate backwards for 1 minute, wherein the rotation is used as a ball milling cycle, and then a plurality of ball milling cycles are carried out;
and step three, unloading the ball milling tank after ball milling is finished, introducing air for 15 minutes, standing for 24 hours, and taking materials to obtain the spherical high-activity aluminum-titanium mechanical alloy powder.
The further technical scheme is that the grinding balls in the first step are stainless steel balls, the sizes of the stainless steel balls are 3mm and 5mm, and the mass ratio of the 3mm stainless steel balls to the 5mm stainless steel balls is 1: 1.
And the further technical scheme is that in the second step, the ball mill is stopped to cool for 30 minutes after each ball milling time of 2 hours.
The further technical scheme is that the total ball milling time in the second step is 40 hours, wherein the cooling time is not included.
Compared with the prior art, the invention has the following beneficial effects:
1. the aluminum-titanium alloy powder prepared by the invention has small grain diameter and average grain size d50Is lower than8.05 μm, minimum mean particle size d50The particle size reaches 6.22 mu m, and the mixing uniformity and the packing density of the medicament can be improved.
2. The micro-morphology of the aluminum-titanium alloy powder prepared by the invention is spherical particles.
3. The aluminum-titanium alloy powder prepared by the invention is amorphous, and diffraction peaks of metal aluminum and metal titanium are completely absent in an XRD (X-ray diffraction) spectrum.
4. The aluminum-titanium alloy powder prepared by the invention has very high activity, the thermal reaction temperature does not exceed 845 ℃, and the lowest thermal reaction temperature reaches 565 ℃; and the thermal reaction temperature of the raw aluminum powder is more than 995 ℃.
5. The aluminum-titanium alloy powder prepared by the invention has very high packing density which is not less than 2.89g/cm3(92% theoretical density), the maximum packing density can reach 3.03g/cm3(94% theoretical density); the loading density of the raw aluminum powder is only 2.37g/cm3(88% theoretical density).
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) photograph of an aluminum-titanium mechanical alloy powder prepared in example 2.
FIG. 2 is a graph of the particle size distribution of the aluminum titanium mechanical alloy powder prepared in example 2.
FIG. 3 is an X-ray diffraction (XRD) pattern of the aluminum-titanium mechanical alloy powder prepared in example.
FIG. 4 shows thermal analysis (DSC) spectra of the Al powder as the raw material and the mechanical alloy powder of Al and Ti prepared in the examples.
FIG. 5 is a Scanning Electron Microscope (SEM) photograph of the aluminum-titanium mechanical alloy powder prepared in comparative example 1.
FIG. 6 is a graph of the particle size distribution of an aluminum-titanium mechanical alloy powder prepared in comparative example 1.
Detailed Description
The present invention will be further described with reference to specific examples, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
Putting 7g of aluminum powder, 3g of titanium powder, 0.8g of stearic acid and 400g of stainless steel balls into a ball milling tank, and uniformly stirring. Wherein the stainless steel ball has a diameter of 200g3mm stainless steel balls and 200g stainless steel balls with a diameter of 5 mm. Setting the running program of the ball mill to rotate forwards for 1 minute, then rotate backwards for 1 minute, rotate forwards for 1 minute, rotate backwards for 1 minute, and so on. The ball mill is started, and the machine is stopped and cooled for 30 minutes every 2 hours of operation. The ball mill was stopped after 40 hours (not including the cooling time). After the ball milling is finished, the ball milling tank is detached, air is introduced for 15 minutes, the ball milling tank is placed for 24 hours, then the material is taken, the spherical high-activity aluminum-titanium mechanical alloy powder is obtained, and the average particle size d of the spherical high-activity aluminum-titanium mechanical alloy powder obtained in the embodiment is50It was 8.05. mu.m.
Taking raw aluminum powder (average particle size d)5050 μm) and the aluminum-titanium mechanical alloy powder prepared in example 1 were tested for thermal reaction temperature, respectively, and the specific steps for testing the thermal reaction temperature (i.e. obtaining a DSC pattern) were as follows: respectively taking 2 mg-5 mg of raw aluminum powder and the aluminum-titanium mechanical alloy powder prepared in the example 2, and adding Al into the raw aluminum powder2O3Placing the micro crucible into a heating chamber of a thermal analyzer (manufactured by Shimadzu corporation, Japan), sealing the heating chamber, opening an air inlet valve, and introducing air into the heating chamber at an air flow rate of 20 mL/min; then setting the temperature rise rate to be 20 ℃/min and setting the temperature rise interval to be 100-1000 ℃ on an operation panel; after the test is finished, the starting button is started, the heating device starts to heat, and the instrument starts to normally test. In the testing process, the instrument is connected with a computer to record the temperature and the heat flow in the micro crucible in real time. When the temperature reaches the set maximum temperature (1000 ℃), the instrument automatically turns off the heating device, automatically turns on the heating chamber to dissipate heat, and the data obtained by the test is automatically stored in a computer connected with the instrument. The data in the computer were taken out to obtain the heat flows at different temperatures, and the temperature T and heat flows were plotted to obtain the DSC chart as in FIG. 4. Taking the peak temperature of the exothermic peak in the DSC spectrogram as the temperature of the thermal reaction, wherein the DSC spectrogram in figure 4 shows that the temperature of the exothermic peak of the thermal reaction of the aluminum-titanium mechanical alloy powder prepared in the example 1 is 845 ℃; the aluminum powder has no exothermic peak at 995 deg.c, i.e., its exothermic peak temperature is > 995 deg.c. In addition, the raw aluminum powder also has melting endothermic phenomenon at 660 ℃, but the aluminum-titanium mechanical alloy powder prepared in the example 1 has no melting endothermic phenomenon. These two points are saidObviously, the activity of the aluminum-titanium mechanical alloy powder is obviously higher than that of the aluminum powder serving as the raw material.
Example 2
Putting 7g of aluminum powder, 3g of titanium powder, 1.0g of stearic acid and 400g of stainless steel balls into a ball milling tank, and uniformly stirring. Wherein the stainless steel ball consists of 200g of stainless steel balls with the diameter of 3mm and 200g of stainless steel balls with the diameter of 5 mm. Setting the running program of the ball mill to rotate forwards for 1 minute, then rotate backwards for 1 minute, rotate forwards for 1 minute, rotate backwards for 1 minute, and so on. The ball mill is started, and the machine is stopped and cooled for 30 minutes every 2 hours of operation. The ball mill was stopped after 40 hours (not including the cooling time). And (4) unloading the ball milling tank after ball milling is finished, introducing air for 15 minutes, standing for 24 hours, and taking the material to obtain the spherical high-activity aluminum-titanium mechanical alloy powder.
The SEM photograph of fig. 1 shows that the aluminum titanium mechanical alloy powder prepared in example 2 has a micro-morphology of spherical particles. FIG. 2 is a particle size distribution diagram showing the average particle size d of the aluminum-titanium mechanical alloy powder prepared in example 2507.84 μm, the grade of the ultrafine powder is reached.
The thermal reaction temperature of the aluminum-titanium mechanical alloy powder prepared in example 2 is measured, and as shown in the DSC chart of FIG. 4, the thermal reaction exothermic peak temperature of the aluminum-titanium mechanical alloy powder prepared in example 2 is 790 ℃, and the exothermic peak temperature of the raw aluminum powder is more than 995 ℃. The activity of the aluminum-titanium mechanical alloy powder is obviously higher than that of the raw aluminum powder.
Example 3
Putting 7g of aluminum powder, 3g of titanium powder, 1.2g of stearic acid and 400g of stainless steel balls into a ball milling tank, and uniformly stirring. Wherein the stainless steel ball consists of 200g of stainless steel balls with the diameter of 3mm and 200g of stainless steel balls with the diameter of 5 mm. Setting the running program of the ball mill to rotate forwards for 1 minute, then rotate backwards for 1 minute, rotate forwards for 1 minute, rotate backwards for 1 minute, and so on. The ball mill is started, and the machine is stopped and cooled for 30 minutes every 2 hours of operation. The ball mill was stopped after 40 hours (not including the cooling time). After the ball milling is finished, the ball milling tank is detached, air is introduced for 15 minutes, the ball milling tank is placed for 24 hours, then the material is taken, the spherical high-activity aluminum-titanium mechanical alloy powder is obtained, and the average particle size d of the spherical high-activity aluminum-titanium mechanical alloy powder obtained in the embodiment is50It was 6.22 μm.
The thermal reaction temperature of the aluminum-titanium mechanical alloy powder prepared in example 3 is measured, and as shown in the DSC chart of FIG. 4, the aluminum-titanium mechanical alloy powder prepared in example 3 has a thermal reaction exothermic peak at 565 ℃, and the exothermic peak temperature of the raw aluminum powder is more than 995 ℃. The activity of the aluminum-titanium mechanical alloy powder is obviously higher than that of the raw aluminum powder.
Comparative example 1
Putting 7g of aluminum powder, 3g of titanium powder, 0.3g of stearic acid and 400g of stainless steel balls into a ball milling tank, and uniformly stirring. Wherein the stainless steel ball consists of 200g of stainless steel balls with the diameter of 3mm and 200g of stainless steel balls with the diameter of 5 mm. Setting the running program of the ball mill to rotate forwards for 30 minutes, then rotate backwards for 30 minutes, rotate forwards for 30 minutes, rotate backwards for 30 minutes, and then circulate in such a way. The ball mill is started, and the machine is stopped and cooled for 30 minutes every 2 hours of operation. The ball mill was stopped after 40 hours (not including the cooling time). And (4) unloading the ball milling tank after ball milling is finished, introducing air for 15 minutes, standing for 24 hours, and taking the material to obtain the aluminum-titanium mechanical alloy powder.
The XRD pattern of FIG. 3 shows that example 1-
3, the aluminum-titanium mechanical alloy powder prepared in the step (3) is all in an amorphous state, and diffraction peaks of metal aluminum powder and metal titanium powder do not appear in an XRD (X-ray diffraction) spectrum.
The SEM photograph of FIG. 5 shows that the sample prepared in comparative example 1 has a microscopic morphology of flaky irregular particles and a large size, and the morphology is significantly different from that of the spherical aluminum-titanium mechanical alloy powder prepared in example 2. This indicates that the stearic acid content significantly affects the micro-morphology of the product.
FIG. 6 is a particle size distribution diagram showing that the average particle size of the samples prepared in comparative example 1 reaches d5022.29 μm, which is significantly larger than the average particle size of the spherical mechanical alloy powder prepared in examples 1-3. The particle size distribution is very wide and reaches 14-36 mu m (the span is 22 mu m); whereas the particle size distribution of the spherical mechanical alloy powder prepared in example 2 was only 3 μm to 15 μm (span 12 μm). This indicates that the content of stearic acid, in addition to affecting the microscopic morphology of the product, also significantly affects the particle size and particle size distribution of the product.
The difference between comparative example 1 and examples 1 to 3 in the preparation process is mainly two points: (1) the stearic acid content in comparative example 1 was low; (2) the procedure for the operation of the ball mill in comparative example 1 was different from that in examples 1 to 3. This shows that in the process of preparing the spherical high-activity aluminum-titanium mechanical alloy powder, the content of stearic acid and the operation program of the ball mill have important influence on the micro-morphology and the granularity of the product.
The aluminum-titanium mechanical alloy powder prepared by the invention can be used as an ignition charge of a combustion bomb, when the aluminum-titanium mechanical alloy powder prepared by the embodiment of the invention is mixed with other raw materials to prepare the combustion bomb, the packing density of the combustion bomb needs to be ensured, and the test method of the packing density comprises the following steps: a certain mass of the aluminum-titanium alloy powder (or the raw aluminum powder) prepared in the examples 1 to 3 and the comparative example 1 is put into a mold and is pressed and molded under a hydraulic press at a pressure of 1 ton, and the molded sample is a standard cylinder. Then, measuring the section diameter and the height of the sample cylinder by using a vernier caliper, and calculating the volume of the cylinder; weighing the mass of the sample cylinder on an electronic balance; then, the actual density of the sample cylinder is calculated according to the formula "density-volume/mass". This density is the packing density of the medicament. The theoretical density of the medicament is calculated according to a method in military mixed explosives, and the detailed method and parameters are shown in documents: military mixed explosive [ M ] bin]Weapon industry Press, 1995, pp.69-70; the test results are shown in the table, and the test results of the packing density from Table 1 show that the products produced in examples 1 to 3 of the present invention had the highest packing density of 3.03g/cm after compaction394% of theoretical density is achieved; the minimum density is 2.89g/cm392% of the theoretical density is achieved. The filling density of the compacted raw aluminum powder is 2.47g/cm3And 88% of theoretical density. The compacted product of comparative example 1 had a packing density of only 2.16g/c m3Only 67% of the theoretical density. This further illustrates that spheronization, small particle size, narrow particle size distribution has a very large effect on drug loading density. The higher the degree of spheronization, the smaller the particle size and the narrower the particle size distribution, the higher the packing density.
TABLE 1 Properties of the products prepared in the examples of the invention
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (1)
1. A preparation method of spherical high-activity aluminum-titanium mechanical alloy powder is characterized by comprising the following steps:
taking aluminum powder, titanium powder and stearic acid, adding the aluminum powder, the titanium powder and the stearic acid and grinding balls into a ball mill, wherein the mass ratio of the grinding balls to materials is 34-38: 1, and uniformly stirring;
starting the ball mill, enabling the ball mill to rotate forwards for 1 minute and then rotate backwards for 1 minute, and then rotate forwards for 1 minute and then rotate backwards for 1 minute, wherein the rotation is used as a ball milling cycle, and then a plurality of ball milling cycles are carried out;
step three, unloading the ball milling tank after ball milling is finished, introducing air for 15 minutes, standing for 24 hours, and then taking materials to obtain spherical high-activity aluminum-titanium mechanical alloy powder;
the spherical high-activity aluminum-titanium mechanical alloy powder is prepared by ball milling the following raw materials in percentage by mass: 62-65% of aluminum powder, 26-28% of titanium powder and 7-11% of stearic acid, wherein the average particle size d50 of the spherical high-activity aluminum-titanium mechanical alloy powder is less than 10 mu m;
the ball mill in the first step is a planetary ball mill;
the grinding balls in the first step are stainless steel balls, the sizes of the grinding balls are 3mm and 5mm, and the mass ratio of the 3mm stainless steel balls to the 5mm stainless steel balls is 1: 1;
stopping cooling the ball mill for 30 minutes after each ball milling time of 2 hours in the step II;
the total ball milling time in the second step is 40 hours, wherein the cooling time is not included.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810581794.3A CN108555282B (en) | 2018-06-07 | 2018-06-07 | Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810581794.3A CN108555282B (en) | 2018-06-07 | 2018-06-07 | Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108555282A CN108555282A (en) | 2018-09-21 |
CN108555282B true CN108555282B (en) | 2020-05-05 |
Family
ID=63553241
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810581794.3A Expired - Fee Related CN108555282B (en) | 2018-06-07 | 2018-06-07 | Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108555282B (en) |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN114082967A (en) * | 2020-08-06 | 2022-02-25 | 北京理工大学 | Preparation method of aluminum-titanium-based multi-component alloy powder and obtained alloy powder |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56133402A (en) * | 1980-02-22 | 1981-10-19 | Western Electric Co | Magnet produced by powder metallurgical treatment |
CN1337377A (en) * | 2001-09-20 | 2002-02-27 | 山东大学 | Intermatallic Ti-Al compound/alumina ceramic composite material and its prepn process |
CN101505893A (en) * | 2006-07-20 | 2009-08-12 | 钛坦诺克斯发展有限公司 | Metal alloy powders production |
CN101524754A (en) * | 2009-04-17 | 2009-09-09 | 中南大学 | Rapid thermal pressed sintering molding process for titanium-aluminum alloy targets |
CN107573202A (en) * | 2017-10-13 | 2018-01-12 | 南京理工大学 | A kind of high-energy combustion agent and preparation method thereof |
CN107653424A (en) * | 2017-11-16 | 2018-02-02 | 康硕电气集团有限公司 | A kind of Ti Al based amorphous alloy powders material, preparation method and applications |
-
2018
- 2018-06-07 CN CN201810581794.3A patent/CN108555282B/en not_active Expired - Fee Related
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS56133402A (en) * | 1980-02-22 | 1981-10-19 | Western Electric Co | Magnet produced by powder metallurgical treatment |
CN1337377A (en) * | 2001-09-20 | 2002-02-27 | 山东大学 | Intermatallic Ti-Al compound/alumina ceramic composite material and its prepn process |
CN101505893A (en) * | 2006-07-20 | 2009-08-12 | 钛坦诺克斯发展有限公司 | Metal alloy powders production |
CN101524754A (en) * | 2009-04-17 | 2009-09-09 | 中南大学 | Rapid thermal pressed sintering molding process for titanium-aluminum alloy targets |
CN107573202A (en) * | 2017-10-13 | 2018-01-12 | 南京理工大学 | A kind of high-energy combustion agent and preparation method thereof |
CN107653424A (en) * | 2017-11-16 | 2018-02-02 | 康硕电气集团有限公司 | A kind of Ti Al based amorphous alloy powders material, preparation method and applications |
Non-Patent Citations (1)
Title |
---|
Particle combustion rates for mechanically alloyed Al-Ti and aluminum powders burning in air;Yuriy L.Shoshin,Edward L.Dreizin;《Combustion and Flame》;20060630;第714-722页 * |
Also Published As
Publication number | Publication date |
---|---|
CN108555282A (en) | 2018-09-21 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN105441765B (en) | Bullet high-specific gravity tungsten alloy and preparation method thereof | |
Schoenitz et al. | Preparation of energetic metastable nano-composite materials by arrested reactive milling | |
CN108555282B (en) | Spherical high-activity aluminum-titanium mechanical alloy powder and preparation method thereof | |
Alshataif et al. | Synthesis, structure, and mechanical response of Cr0. 26Fe0. 24Al0. 5 and Cr0. 15Fe0. 14Al0. 30Cu0. 13Si0. 28 nanocrystallite entropy alloys | |
Dong et al. | Fabrication of intermetallic NiAl by self-propagating high-temperature synthesis reaction using aluminium nanopowder under high pressure | |
CN101210291B (en) | Method for producing ultra-fine crystal particle cermet | |
CN107721783B (en) | A kind of boron magnesium prealloy powder body material and preparation method thereof | |
US20210032741A1 (en) | Fe-Pt-OXIDE-BN-BASED SINTERED COMPACT FOR SPUTTERING TARGET | |
JP2002501440A (en) | Prealloyed copper-containing powder and its use in the production of diamond tools | |
CN108281245A (en) | A kind of preparation method of samarium cobalt permanent magnet body | |
Jiao et al. | Effect of fluoropolymer content on thermal and combustion performance of direct writing high-solid nanothermite composite | |
CN110343905A (en) | High-temperature titanium alloy and preparation method thereof | |
Mwamba et al. | The use of titanium hydride in blending and mechanical alloying of Ti-Al alloys | |
KR101235081B1 (en) | A magnesium hydride powder and Manufacturing process of magnesium hydride powder by heat treatment under the pressure in hydrogen atmosphere of ball milled magnesium powder | |
Neves et al. | Mechanically activated reactive forging synthesis (MARFOS) of NiTi | |
Song et al. | Mechanical alloying of FeAl intermetallic powder for metal injection moulding process | |
Gülsoy et al. | Injection molding of mechanical alloyed Ti–Fe–Zr powder | |
CN102560167A (en) | Aluminum alloy and preparation method thereof | |
CN1118584C (en) | Process for preparing W-Ni-Fe alloy with superfine grains and high specific weight | |
Pourhosseini et al. | Preparation of FeAl–Al2O3 nanocomposite via mechanical alloying and subsequent annealing | |
An et al. | Preparation, Characterization, and Application of Superthermites in Solid Propellant | |
RU2447177C1 (en) | Method of producing modifying agent for nickel alloys | |
CN110560697A (en) | preparation process for producing cobalt-base alloy powder metallurgy by simple substance ball milling method | |
CN109834272A (en) | A kind of hot isostatic pressing FGH4169 alloy | |
CN113025859B (en) | High-strength high-plasticity tungsten alloy material and preparation method thereof |
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 | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20200505 |