CN112094163A - Nano-scale aluminum/polytetrafluoroethylene active material and preparation process thereof - Google Patents
Nano-scale aluminum/polytetrafluoroethylene active material and preparation process thereof Download PDFInfo
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- CN112094163A CN112094163A CN202011027365.5A CN202011027365A CN112094163A CN 112094163 A CN112094163 A CN 112094163A CN 202011027365 A CN202011027365 A CN 202011027365A CN 112094163 A CN112094163 A CN 112094163A
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
- C06B21/0033—Shaping the mixture
- C06B21/0041—Shaping the mixture by compression
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B21/00—Apparatus or methods for working-up explosives, e.g. forming, cutting, drying
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B23/00—Compositions characterised by non-explosive or non-thermic constituents
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
- C06B27/00—Compositions containing a metal, boron, silicon, selenium or tellurium or mixtures, intercompounds or hydrides thereof, and hydrocarbons or halogenated hydrocarbons
Abstract
The invention provides a nano-scale aluminum/polytetrafluoroethylene active material and a preparation process thereof, relating to the technical field of energetic materials. A kind of nanometer aluminium/polytetrafluoroethylene active material, such nanometer aluminium/polytetrafluoroethylene active material, improve the active material of aluminium/polytetrafluoroethylene from the grain diameter of raw materials, can improve the dynamic compressive strength of the active material of aluminium/polytetrafluoroethylene apparently, help to promote the use value of the product; in addition, the invention also provides a preparation process of the nano-scale aluminum/polytetrafluoroethylene active material, which comprises the following steps: the preparation of mixed medicinal powder, the pressing of prepared grain, the pressing of quasi-grain and the sintering of grain, the whole preparation process is simple, which is helpful to reduce the cost and the product has high use value.
Description
Technical Field
The invention relates to the field of energetic materials, in particular to a nano-scale aluminum/polytetrafluoroethylene active material and a preparation process thereof.
Background
The aluminum/polytetrafluoroethylene active material is an active material which can generate strong deflagration reaction under the action of impact load/thermal load and release a large amount of chemical energy, belongs to the category of energetic materials, and has the advantage of high energy density compared with the traditional energetic materials such as explosive, propellant, pyrotechnic composition and the like. At present, the material is mainly used in the environments of dynamic loading, penetration and the like, the dynamic mechanical property of the material is mainly determined by soft matrix polytetrafluoroethylene, the compressive strength is low, and the large-area application of the material in weaponry is severely limited.
At present, the existing aluminum/polytetrafluoroethylene active material mainly adopts micron-grade raw materials, and the micron-grade aluminum/polytetrafluoroethylene active material is often poor in dynamic compression strength and low in practicability.
Disclosure of Invention
The invention aims to provide a nanoscale aluminum/polytetrafluoroethylene active material which adopts a nanoscale metal raw material, can greatly improve the dynamic compression strength of the material and has high practicability.
The invention also aims to provide a preparation process of the nano-scale aluminum/polytetrafluoroethylene active material, which has the advantages of simple process flow, contribution to reducing the cost, easy production, convenient use and high practical value.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
In one aspect, the embodiment of the present invention provides a nanoscale aluminum/polytetrafluoroethylene active material, which includes the following raw materials: aluminum powder and polytetrafluoroethylene powder, wherein the particle size of the aluminum powder is 45-55 nm.
On the other hand, the embodiment of the present application provides a preparation process of a nano-scale aluminum/polytetrafluoroethylene active material, which includes the following steps:
preparing mixed medicinal powder: weighing aluminum powder and polytetrafluoroethylene powder in a vacuum glove box, and putting the weighed aluminum powder and polytetrafluoroethylene powder into a stirrer for stirring to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a protective gas environment, putting the die into a press, pressurizing, and pressing the mixed powder by using a punch to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch, further pressing the prepared grain, and demoulding after pressing to obtain a quasi-grain;
sintering the grain: and (3) placing the quasi-explosive column into a crucible, then placing the crucible into a muffle furnace, filling protective gas into the muffle furnace, heating for sintering in a protective gas environment, and cooling after sintering to obtain a finished product.
Compared with the prior art, the embodiment of the invention has at least the following advantages or beneficial effects:
aiming at the first aspect, the embodiment of the invention provides a nanoscale aluminum/polytetrafluoroethylene active material, which comprises the following raw materials: aluminum powder and polytetrafluoroethylene powder, wherein the particle size of the aluminum powder is 45-55 nm.
The nanoscale aluminum/polytetrafluoroethylene active material is improved in terms of particle size of raw materials, aluminum powder with the particle size of 45-55nm is adopted, so that the aluminum powder and polytetrafluoroethylene can be better matched, the material can be pressed more tightly in the subsequent pressing process, and the strength of the aluminum/polytetrafluoroethylene active material is enhanced; through experimental detection, the aluminum powder with the nano-scale particle size is added into the raw materials, so that the dynamic compression strength of the aluminum/polytetrafluoroethylene active material can be obviously improved, and the improvement of the use value of the product is facilitated.
Aiming at the second aspect, the embodiment of the invention provides a preparation method of a nano-scale aluminum/polytetrafluoroethylene active material, which comprises the following steps:
preparing mixed medicinal powder: weighing aluminum powder and polytetrafluoroethylene powder in a vacuum glove box, and putting the weighed aluminum powder and polytetrafluoroethylene powder into a stirrer for stirring to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a protective gas environment, putting the die into a press, pressurizing, and pressing the mixed powder by using a punch to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch, further pressing the prepared grain, and demoulding after pressing to obtain a quasi-grain;
sintering the grain: and (3) placing the quasi-explosive column into a crucible, then placing the crucible into a muffle furnace, filling protective gas into the muffle furnace, heating for sintering in a protective gas environment, and cooling after sintering to obtain a finished product.
According to the preparation process of the nanoscale aluminum/polytetrafluoroethylene active material, firstly, the aluminum powder and the polytetrafluoroethylene powder are fully stirred by a stirrer in the mixed powder preparation step, so that the raw materials are uniformly mixed, the uniform texture of the product is ensured, the performance of the product can be guaranteed, and the use value of the product is favorably improved; through the step of pressing the prepared grains, the raw materials are preliminarily pressed and molded to obtain the prepared grains, so that the subsequent steps are facilitated to further perform pressurization pressing, and meanwhile, the characteristics of the raw materials can be protected from being damaged due to overlarge pressure, and the performance of the product can be improved; through the quasi-drug column pressing step, the prepared drug column is further pressurized and pressed, and then the model is removed to obtain the quasi-drug column, so that the material of the drug column can be pressed more tightly, the performance of a product is further improved, meanwhile, the drug column cannot be damaged due to overlarge pressure, and the use value of the product is favorably improved; through the sintering step of the explosive column, the quasi-explosive column is heated and sintered in a muffle furnace to prepare a finished product, and the components of the explosive column are fully combined at high temperature, so that the performance of the product is further improved, and the use value of the product is improved; the whole preparation process is simple, and the cost is reduced; the aluminum powder with the nano-scale particle size is adopted to modify the aluminum/polytetrafluoroethylene active material, so that the dynamic compression strength of the aluminum/polytetrafluoroethylene active material can be obviously improved, and the product has high use value.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a graph of experimental data for dynamic compression of aluminum/polytetrafluoroethylene materials prepared by conventional processes;
FIG. 2 is a data diagram of a dynamic compression experiment of a nanoscale aluminum/polytetrafluoroethylene material provided in example 7 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to specific examples.
The embodiment of the invention provides a nano-scale aluminum/polytetrafluoroethylene active material, which comprises the following raw materials: aluminum powder and polytetrafluoroethylene powder, wherein the particle size of the aluminum powder is 45-55 nm.
In the embodiment, the aluminum powder with the particle size of 45-55nm is adopted, and the aluminum/polytetrafluoroethylene active material is improved in the aspect of the particle size of the raw materials, so that the aluminum powder and the polytetrafluoroethylene powder can be better matched, and the material can be pressed more tightly in the subsequent pressing process, and the strength of the aluminum/polytetrafluoroethylene active material is enhanced; through experimental detection, the aluminum powder with the nano-scale particle size is added into the raw materials, so that the dynamic compression strength of the aluminum/polytetrafluoroethylene active material can be obviously improved, and the improvement of the use value of the product is facilitated.
In some embodiments of the present invention, the particle size of the polytetrafluoroethylene powder is 30 to 35 μm.
In the embodiment, the polytetrafluoroethylene powder with the particle size of 30-35 microns is adopted, so that the polytetrafluoroethylene powder can be better matched with the aluminum powder with the nano-scale particle size, the material can be pressed and combined more tightly and sufficiently in the subsequent process, the product performance is improved, gaps cannot be generated in the material due to too large particle size, the product performance cannot be influenced due to too small particle size, and the product has high use value.
In some embodiments of the present invention, the aluminum powder is used in an amount of 25 to 30 parts by weight, and the polytetrafluoroethylene powder is used in an amount of 70 to 75 parts by weight.
In the embodiment, the use performance of the product can be ensured by adopting the weight ratio, the influence on the product performance caused by too much or too little raw material parts is avoided, and meanwhile, the ratio is favorable for better matching among materials, so that the product performance is improved, and the practical value of the product can be improved.
The embodiment of the invention also provides a preparation process of the nano-scale aluminum/polytetrafluoroethylene active material, which comprises the following steps:
preparing mixed medicinal powder: weighing aluminum powder and polytetrafluoroethylene powder in a vacuum glove box, and putting the weighed aluminum powder and polytetrafluoroethylene powder into a stirrer for stirring to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a protective gas environment, putting the die into a press, pressurizing, and pressing the mixed powder by using a punch to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch, further pressing the prepared grain, and demoulding after pressing to obtain a quasi-grain;
sintering the grain: and (3) placing the quasi-explosive column into a crucible, then placing the crucible into a muffle furnace, filling protective gas into the muffle furnace, heating for sintering in a protective gas environment, and cooling after sintering to obtain a finished product.
In the embodiment, the aluminum powder, the polytetrafluoroethylene powder and the zirconium wire whiskers are fully and uniformly mixed through the mixed raw material preparation step, so that the uniformity of the texture of the product is ensured, the material characteristics are ensured, the product performance is ensured, and the practical value of the product is improved; through the powder column pressing step, the pressurization rate is controlled to press the mixed powder into the powder column, so that the characteristics of the raw materials can be prevented from being damaged due to overlarge pressure, and the raw materials can be pressed and combined more tightly, thereby improving the dynamic compression strength of the product and improving the practical value of the product; through the sintering step of the explosive columns, the temperature rise rate of the muffle furnace is controlled to sinter the explosive columns, so that the performance of the explosive columns can be prevented from being damaged due to overhigh temperature, and the sintering of the explosive columns can be more compact and sufficient, thereby further improving the dynamic compression strength of the product and further enhancing the practical value of the product; the process is improved by taking zirconium wire whiskers as the filler and improving the aluminum/polytetrafluoroethylene active material, the impact reaction energy release capacity of the aluminum/polytetrafluoroethylene active material cannot be influenced, the whole process flow is simple, the production cost is favorably reduced, the production is easy, and the produced product has high dynamic compression strength and high practical value through experimental detection.
In some embodiments of the present invention, in the powder mixing step, the mixer is operated at a rotation speed of 8-12r/s for 5-10 minutes to obtain the mixed powder.
In the embodiment, the stirring machine can stir at the rotating speed of 8-12r/s for 5-10 minutes, so that the raw materials can be stirred and mixed uniformly at the stirring speed and the stirring time, the texture uniformity of the product is ensured, the product performance is improved, the raw materials can be prevented from being damaged due to too high rotating speed and too long time, and the use value of the product is further improved.
In some embodiments of the present invention, in the preliminary drug column pressing step, the punch presses the mixed powder to 30-35MPa at a pressure increasing speed of 60-65MPa/min, so as to obtain a preliminary drug column.
In the embodiment, the punch is controlled to be pressurized to 30-35MPa at the pressure increasing speed of 60-65MPa/min, so that the mixed medicinal powder can be initially pressed into the preparation medicinal column, and the mixed medicinal powder can be prevented from being damaged due to too high pressurizing speed and too high pressure, the product performance is ensured, and the use value of the product is improved.
In some embodiments of the invention, in the quasi-drug column pressing step, the punch is pressurized to 30-35MPa at a pressure increasing speed of 60-65MPa/Min, then pressurized to 480-510MPa at a pressure increasing speed of 130-160MPa/Min, and subjected to pressure maintaining of 5-10Min, and the quasi-drug column is obtained after demolding.
In the embodiment, the punch is controlled to be pressurized to 30-35MPa at the boosting speed of 60-65MPa/Min, then pressurized to 480-510MPa at the boosting speed of 130-160MPa/Min, and the pressure is maintained for 5-10Min, so that the prepared grain can be prevented from being damaged due to too high boosting speed and too high pressure while the upper prepared grain is further pressed into the standard grain, the product performance is ensured, and the use value of the product is improved.
In some embodiments of the invention, in the step of sintering the pillars, the muffle furnace is filled with a protective gas, the flow rate of the protective gas is 20-30L/min, the muffle furnace is heated to 350 ℃ with a temperature rise rate of 1-1.5 ℃/min, then heated to 400 ℃ with a temperature rise rate of 0.5-1 ℃/min, and then is kept warm for 30-60min, and then is cooled to 300 ℃ with a temperature fall rate of 0.5-1 ℃/min, and is kept warm for 30-60min, then is cooled to 100-90 ℃ with a temperature fall rate of 1.5-2 ℃/min, and finally is naturally cooled to room temperature in the muffle furnace, so as to obtain the finished product.
In the embodiment, the protective gas is filled into the muffle furnace, the flow of the protective gas is 20-30L/min, the protective gas can prevent the quasi-explosive columns from being polluted by impurities in the sintering process, and meanwhile, the protective gas can also play a role in heat conduction, so that the components of the quasi-explosive columns can be fully sintered, and the performance of products can be further improved; the method comprises the steps of controlling a muffle furnace to heat up to 350 ℃ in a temperature rise rate of 1-1.5 ℃/min, then heating up to 400 ℃ in a temperature rise rate of 0.5-1 ℃/min, preserving heat for 30-60min, then cooling to 300 ℃ in a temperature rise rate of 350 ℃ in a temperature rise rate of 0.5-1 ℃/min, preserving heat for 30-60min, then cooling to 100-90 ℃ in a temperature fall rate of 1.5-2 ℃/min, and finally naturally cooling to room temperature, further sintering the quasi-drug column to obtain a finished product, completely combining the components of the quasi-drug column together through high temperature, further improving the performance of the product, protecting the quasi-drug column from being damaged due to too high temperature and too high temperature, and being beneficial to improving the use value of the product.
In some embodiments of the present invention, the protective gas is nitrogen.
In the embodiment, the nitrogen gas can be used for better protecting, and meanwhile, the nitrogen gas can also have the heat conducting effect, and the nitrogen gas heat conduction device is convenient to use.
In some embodiments of the invention, the press is a YLJ-50 vertical press.
In the embodiment, the YLJ-50 vertical press can better control the pressing pressure, is convenient to use and is beneficial to pressing.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: weighing 30g of aluminum powder with the particle size of 55nm and 75g of polytetrafluoroethylene powder with the particle size of 35 microns in a vacuum glove box, putting the weighed aluminum powder and polytetrafluoroethylene into a stirrer, stirring at the rotating speed of 12r/s for 10 minutes to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 35MPa by a punch at a pressurizing speed of 65MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 35MPa at a pressure increasing speed of 65MPa/Min, then pressurizing to 510MPa at a pressure increasing speed of 160MPa/Min, maintaining the pressure for 5-10Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 30L/min, heating the muffle furnace to 350 ℃ at a temperature rise rate of 1.5 ℃/min in a nitrogen environment, heating to 400 ℃ at a temperature rise rate of 1 ℃/min, preserving heat for 60min, cooling to 350 ℃ at a temperature reduction rate of 1 ℃/min, preserving heat for 60min, cooling to 100 ℃ at a temperature reduction rate of 2 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain a finished product.
Example 2
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: weighing 25g of aluminum powder with the particle size of 45nm and 70g of polytetrafluoroethylene powder with the particle size of 30 microns in a vacuum glove box, putting the weighed aluminum powder and polytetrafluoroethylene into a stirrer, stirring at the rotating speed of 8r/s for 5 minutes to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 30MPa by a punch at a pressurizing speed of 60MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 30MPa at a pressurizing speed of 60MPa/Min, then pressurizing to 480MPa at a pressurizing speed of 130MPa/Min, maintaining the pressure for 5Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 20L/min, heating the muffle furnace to 300 ℃ at the temperature rise rate of 1 ℃/min, heating to 350 ℃ at the temperature rise rate of 0.5 ℃/min in a nitrogen environment, preserving heat for 30min, cooling to 300 ℃ at the temperature reduction rate of 0.5 ℃/min, preserving heat for 30min, cooling to 90 ℃ at the temperature reduction rate of 1.5 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain a finished product.
Example 3
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: 27g of aluminum powder with the particle size of 50nm and 73g of polytetrafluoroethylene powder with the particle size of 32 microns are weighed in a vacuum glove box, the weighed aluminum powder and polytetrafluoroethylene are put into a stirrer to be stirred at the rotating speed of 10r/s for 8 minutes, and mixed powder is obtained;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 35MPa by a punch at a pressurizing speed of 63MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 35MPa at a pressurizing speed of 62MPa/Min, then pressurizing to 500MPa at a pressurizing speed of 145MPa/Min, maintaining the pressure for 8Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 25L/min, heating the muffle furnace to 325 ℃ at the temperature rise rate of 1.3 ℃/min in a nitrogen environment, heating to 380 ℃ at the temperature rise rate of 0.8 ℃/min, preserving heat for 45min, cooling to 325 ℃ at the temperature fall rate of 0.8 ℃/min, preserving heat for 45min, cooling to 95 ℃ at the temperature fall rate of 1.5 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain the finished product.
Example 4
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: 26g of aluminum powder with the particle size of 48nm and 72g of polytetrafluoroethylene powder with the particle size of 32 microns are weighed in a vacuum glove box, the weighed aluminum powder and polytetrafluoroethylene are put into a stirrer to be stirred at the rotating speed of 10r/s for 5 minutes, and mixed powder is obtained;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 32MPa by a punch at a pressurizing speed of 62MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 32MPa at a boosting speed of 62MPa/Min, then pressurizing to 490MPa at a boosting speed of 140MPa/Min, maintaining the pressure for 6Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 20L/min, heating the muffle furnace to 310 ℃ at the temperature rise rate of 1.2 ℃/min in a nitrogen environment, heating to 360 ℃ at the temperature rise rate of 0.8 ℃/min, preserving heat for 40min, cooling to 310 ℃ at the temperature reduction rate of 0.8 ℃/min, preserving heat for 40min, cooling to 90 ℃ at the temperature reduction rate of 1.6 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain a finished product.
Example 5
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: weighing 28g of aluminum powder with the particle size of 52nm and 74g of polytetrafluoroethylene powder with the particle size of 32 mu m in a vacuum glove box, putting the weighed aluminum powder and polytetrafluoroethylene into a stirrer, stirring at the rotating speed of 12r/s, and stirring for 10 minutes to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 35MPa by a punch at a pressurizing speed of 65MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 35MPa at a pressure increasing speed of 65MPa/Min, then pressurizing to 500MPa at a pressure increasing speed of 150MPa/Min, maintaining the pressure for 8Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 30L/min, heating the muffle furnace to 340 ℃ at the temperature rise rate of 1.4 ℃/min in a nitrogen environment, heating to 390 ℃ at the temperature rise rate of 0.8 ℃/min, preserving heat for 50min, cooling to 340 ℃ at the temperature reduction rate of 0.8 ℃/min, preserving heat for 50min, cooling to 95 ℃ at the temperature reduction rate of 1.8 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain the finished product.
Example 6
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: 26.5g of aluminum powder with the particle size of 50nm and 73.5g of polytetrafluoroethylene powder with the particle size of 34 mu m are weighed in a vacuum glove box, the weighed aluminum powder and the weighed polytetrafluoroethylene are put into a stirrer to be stirred at the rotating speed of 8r/s for 10 minutes to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 35MPa by a punch at a pressurizing speed of 60MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 35MPa at a pressurizing speed of 60MPa/Min, then pressurizing to 480MPa at a pressurizing speed of 140MPa/Min, maintaining the pressure for 10Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 30L/min, heating the muffle furnace to 340 ℃ at a temperature rise rate of 1.2 ℃/min in a nitrogen environment, heating to 400 ℃ at a temperature rise rate of 1 ℃/min, preserving heat for 60min, cooling to 340 ℃ at a temperature reduction rate of 1 ℃/min, preserving heat for 60min, cooling to 100 ℃ at a temperature reduction rate of 2 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain a finished product.
Example 7
The embodiment provides a nanoscale aluminum/polytetrafluoroethylene active material, which is prepared by the following steps:
preparing mixed medicinal powder: 26.5g of aluminum powder with the particle size of 50nm and 73.5g of polytetrafluoroethylene powder with the particle size of 34 mu m are weighed in a vacuum glove box, the weighed aluminum powder and the weighed polytetrafluoroethylene are put into a stirrer to be stirred at the rotating speed of 12r/s for 5 minutes to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a nitrogen environment, putting the die into a press, pressurizing, and pressurizing the mixed powder to 30MPa by a punch at a pressurizing speed of 60MPa/min to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch to 30MPa at a pressurizing speed of 60MPa/Min, then pressurizing to 500MPa at a pressurizing speed of 150MPa/Min, maintaining the pressure for 5Min, further pressing the prepared grain, and demolding after pressing to obtain a quasi-grain;
sintering the grain: and (2) placing the quasi-drug column into a crucible, placing the crucible into a muffle furnace, filling nitrogen into the muffle furnace, wherein the nitrogen flow is 20L/min, heating the muffle furnace to 325 ℃ at the temperature rise rate of 1.3 ℃/min in a nitrogen environment, heating to 360 ℃ at the temperature rise rate of 0.7 ℃/min, preserving heat for 30min, cooling to 325 ℃ at the temperature reduction rate of 0.6 ℃/min, preserving heat for 30min, cooling to 100 ℃ at the temperature reduction rate of 1.9 ℃/min, and naturally cooling to room temperature in the muffle furnace to obtain a finished product.
Test examples
The aluminum/polytetrafluoroethylene active material prepared by the traditional formula process is subjected to dynamic compression experiment through a Hopkinson experiment system, the Hopkinson pressure bar is made of solid solution reinforced aluminum, and the loading strain rate is 3000s-1The measured data are shown in fig. 1.
The dynamic compression experiment is carried out on the nano-scale aluminum/polytetrafluoroethylene active material provided by the embodiment 7 of the invention through a Hopkinson experiment system, the Hopkinson pressure bar is made of solid solution strengthened aluminum, and the loading strain rate is 3000s-1The measured data are shown in fig. 2.
As can be seen from FIG. 1, the dynamic compressive strength of the aluminum/PTFE material prepared by the conventional formulation process is 54.8MPa, and the maximum strain is 0.25.
As can be seen from fig. 2, the nanoscale aluminum/polytetrafluoroethylene active material provided in example 7 of the present invention has a dynamic compressive strength of 90MPa and a maximum strain of 0.006.
As can be seen from the comparison between FIG. 1 and FIG. 2, the dynamic compressive strength of the nano-scale aluminum/polytetrafluoroethylene active material provided by the invention is far higher than that of the aluminum/polytetrafluoroethylene active material prepared by the traditional process, and the product performance and the use value are high.
In summary, the nanoscale aluminum/polytetrafluoroethylene active material and the preparation process thereof provided by the embodiment of the invention improve the aluminum/polytetrafluoroethylene active material from the aspect of particle size of raw materials, and by adopting the aluminum powder with the particle size of 45-55nm, the aluminum powder and the polytetrafluoroethylene can be better matched, so that the material can be pressed more tightly in the subsequent pressing process, and the strength of the aluminum/polytetrafluoroethylene active material is enhanced; through experimental detection, the dynamic compression strength of the aluminum/polytetrafluoroethylene active material can be obviously improved by adding the aluminum powder with the nano-scale particle size into the raw materials, and the use value of the product is favorably improved; the preparation process comprises the steps of firstly, fully stirring the aluminum powder and the ground polytetrafluoroethylene powder by a stirrer through the preparation steps of the mixed powder, so that the raw materials are uniformly mixed, thereby ensuring the uniform texture of the product, ensuring the performance of the product and being beneficial to improving the use value of the product; through the step of pressing the prepared grains, the raw materials are preliminarily pressed and molded to obtain the prepared grains, so that the subsequent steps are facilitated to further perform pressurization pressing, and meanwhile, the characteristics of the raw materials can be protected from being damaged due to overlarge pressure, and the performance of the product can be improved; through the quasi-drug column pressing step, the prepared drug column is further pressurized and pressed, and then the model is removed to obtain the quasi-drug column, so that the material of the drug column can be pressed more tightly, the performance of a product is further improved, meanwhile, the drug column cannot be damaged due to overlarge pressure, and the use value of the product is favorably improved; through the sintering step of the explosive column, the quasi-explosive column is heated and sintered in a muffle furnace to prepare a finished product, and the components of the explosive column are fully combined at high temperature, so that the performance of the product is further improved, and the use value of the product is improved; the whole preparation process is simple, and the cost is reduced; the aluminum powder with the nano-scale particle size is adopted to modify the aluminum/polytetrafluoroethylene active material, so that the dynamic compression strength of the aluminum/polytetrafluoroethylene active material can be obviously improved, and the product has high use value.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Claims (10)
1. The nano-scale aluminum/polytetrafluoroethylene active material is characterized by comprising the following raw materials: aluminum powder and polytetrafluoroethylene powder, wherein the particle size of the aluminum powder is 45-55 nm.
2. The nanoscale aluminum/polytetrafluoroethylene active material as set forth in claim 1, wherein the particle size of said polytetrafluoroethylene powder is 30-35 μm.
3. The nanoscale aluminum/polytetrafluoroethylene active material as set forth in claim 2, wherein the aluminum powder is used in an amount of 25-30 parts by weight, and the polytetrafluoroethylene powder is used in an amount of 70-75 parts by weight.
4. A process for preparing nanoscale aluminum/polytetrafluoroethylene active material according to any of claims 1-3, characterized in that it comprises the following steps:
preparing mixed medicinal powder: weighing aluminum powder and polytetrafluoroethylene powder in a vacuum glove box, and putting the weighed aluminum powder and polytetrafluoroethylene powder into a stirrer for stirring to obtain mixed powder;
pressing a prepared grain: putting the mixed powder into a die in a protective gas environment, putting the die into a press, pressurizing, and pressing the mixed powder by using a punch to obtain a prepared powder column;
pressing the quasi-drug column: in an air environment, further pressurizing the punch, further pressing the prepared grain, and demoulding after pressing to obtain a quasi-grain;
sintering the grain: and placing the quasi-explosive column into a crucible, then placing the crucible into a muffle furnace, filling protective gas into the muffle furnace, heating for sintering in a protective gas environment, and cooling after sintering to obtain a finished product.
5. The process for preparing a nano-scale aluminum/polytetrafluoroethylene active material according to claim 4, wherein in the step of mixing the powder, the stirrer is used for stirring at a rotating speed of 8-12r/s for 5-10 minutes to obtain the mixed powder.
6. The process for preparing a nano-scale aluminum/polytetrafluoroethylene active material according to claim 4, wherein in the preliminary drug column pressing step, the punch presses the mixed powder at a pressure increasing speed of 60-65MPa/min to 30-35MPa to obtain a preliminary drug column.
7. The process of claim 4, wherein in the step of pressing the quasi-drug column, the punch is pressurized to 30-35MPa at a pressure increasing rate of 60-65MPa/Min, then pressurized to 480-510MPa at a pressure increasing rate of 130-160MPa/Min, and then pressurized to 5-10Min for mold stripping to obtain the quasi-drug column.
8. The process for preparing a nano-scale aluminum/polytetrafluoroethylene active material according to claim 4, wherein in the step of sintering the pillars, protective gas is filled into a muffle furnace, the flow rate of the protective gas is 20-30L/min, the muffle furnace is heated to 350 ℃ at the temperature rise rate of 1-1.5 ℃/min, then the temperature rise rate of 0.5-1 ℃/min is heated to 400 ℃ at 350 ℃ at the temperature rise rate of 0.5-1 ℃/min, the temperature is maintained for 30-60min, then the temperature is cooled to 300 ℃ at 350 ℃ at the temperature decrease rate of 0.5-1 ℃/min, the temperature is maintained for 30-60min, then the temperature is cooled to 100-90 ℃ at the temperature decrease rate of 1.5-2 ℃/min, and finally the product is obtained by natural cooling to room temperature in the muffle furnace.
9. The process for preparing nano-scale aluminum/polytetrafluoroethylene active material according to claim 4, wherein said protective gas is nitrogen.
10. The process for preparing nano-scale aluminum/polytetrafluoroethylene active material according to claim 4, wherein the press machine is a YLJ-50 vertical press machine.
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