An active material and a preparation method thereof

Abstract

The present invention relates to the technical field of energetic materials, and particularly to an active material and a preparation method thereof. The preparation method of the active material includes: S1: mixing a first metal powder and a second metal powder to obtain a mixed metal powder; S2: performing pressing treatment on the mixed metal powder and then performing vacuum sintering treatment to obtain a metal alloy material; S3: performing hot hydrogen treatment on the metal alloy material to obtain the active material; wherein, the first metal powder is a mixture of a titanium-containing powder and a pure tantalum powder, or a mixture of a titanium-containing powder and a pure zirconium powder; the density of the second metal powder is 15-19.5 g / cm³. By designing the composition of the active material, the present invention can achieve controllability of density and mechanical properties within a certain range; and the active material has sufficient mechanical properties under high-speed impact conditions to ensure integrity, and can also provide sufficient additional chemical energy to improve the damage aftereffect of fragments.

Description

Technical Field

[0001] The present invention relates to the technical field of energetic materials, and particularly to an active material and a preparation method thereof. Background Art

[0002] As the main goal pursued by modern weapon ammunition, traditional inert metal fragments can only damage targets in a pure kinetic energy penetration and perforation manner. Although traditional energetic materials such as explosives, gunpowders, and propellants have the advantages of chemical energy and explosive damage, they lack sufficient strength and can only achieve kinetic energy damage through the release and conversion of chemical energy. The remarkable technical feature of active fragments is that they integrate the advantages of both strength and energy, possessing both the mechanical strength of traditional inert metal fragments and the explosive energy similar to traditional energetic materials, which can significantly improve the damage effect of weapon ammunition.

[0003] According to the characteristics of active fragments, the design of active fragments using high heat of formation metals has gradually attracted attention. Patent CN113651659B invented an aluminum-nickel fragment, which was synthesized by the path of powder mixing - forming - sintering. Although the heat release is high, the density is low; Patent CN115615260B invented a high-density and high heat of formation refractory high-entropy alloy fragment material, including elements such as W, Al, Ti, Zr, Nb, and Ta, and was melted by a non-consumable arc melting method. Each alloy ingot of each component was remelted at least 5 times to ensure the uniformity of chemical composition, which is prone to composition segregation and the process is complex.

[0004] In view of the low density and composition segregation characteristics of the above-mentioned fragments, the present invention is proposed. Summary of the Invention

[0005] Based on this, the present invention has the following technical solutions:

[0006] In a first aspect, the present invention provides a preparation method of an active material, including:

[0007] S1: Mix a first metal powder and a second metal powder to obtain a mixed metal powder;

[0008] S2: Press the mixed metal powder, and then perform vacuum sintering treatment to obtain a metal alloy material;

[0009] S3: Perform hot hydrogen treatment on the metal alloy material to obtain the active material;

[0010] The first metal powder is a mixture of a titanium-containing powder and a pure tantalum powder, or a mixture of a titanium-containing powder and a pure zirconium powder; the titanium-containing powder is a pure titanium powder and / or a titanium alloy powder;

[0011] The density of the second metal powder is 15 - 19.5 g / cm³.

[0012] In the present invention, the density of the second metal powder may specifically be any value among 15 g / cm³, 16 g / cm³, 17 g / cm³, 18 g / cm³, 19.5 g / cm³, or a value range with any two of the above values as endpoints.

[0013] The present invention uses a mixture of a high-density metal and a high heat of formation metal as raw materials, and combines a thermal hydrogen treatment technology to infiltrate hydrogen elements into the fragments, so as to obtain an active fragment with high density and high energy release; when the main components of the active fragment collide at high speed, they react with air to release heat, and the hydrogen in the fragments will also be released and react with oxygen, improving the penetration and damage ability, and is expected to be used as a fragment material.

[0014] Preferably, the second metal powder includes pure tungsten powder.

[0015] Preferably, the titanium alloy powder includes TA15 powder and / or TC4 powder.

[0016] Preferably, the mass ratio of the first metal powder to the second metal powder is (4 - 99):1.

[0017] More preferably, the mass ratio of the first metal powder to the second metal powder is (4 - 20):1.

[0018] In the present invention, the mass ratio of the first metal powder to the second metal powder may be any ratio among 4:1, 5:1, 6:1, 7:1, 8:1, 9:1, 10:1, 11:1, 12:1, 13:1, 14:1, 15:1, 16:1, 17:1, 18:1, 19:1, 20:1, or a ratio range with any two of the above ratios as endpoints.

[0019] Preferably, the first metal powder is composed of a titanium-containing powder and pure tantalum powder with a mass ratio of 1:(1.8 - 8.9); more preferably, the first metal powder is composed of pure titanium powder and pure tantalum powder with a mass ratio of 1:(2 - 8).

[0020] Preferably, the particle size of the first metal powder is 10 - 80 μm; the particle size of the second metal powder is 3 - 20 μm. More preferably, the particle size of the first metal powder is 10 - 60 μm; the particle size of the second metal powder is 5 - 15 μm.

[0021] Preferably, S3 includes performing a thermal hydrogen treatment on the metal alloy material in a hydrogen atmosphere at 500 - 800 °C; preferably, heat preservation is carried out at 550 - 700 °C for 90 - 120 min.

[0022] Preferably, in S3, the flow rate of hydrogen is 0.5 - 3 L / min; more preferably, the flow rate of hydrogen is 0.5 - 2 L / min.

[0023] Preferably, in S2, the conditions for the vacuum sintering treatment include: the sintering temperature is 1200°C - 1500°C; more preferably, sintering is carried out at 1200°C - 1450°C for 120 min - 180 min.

[0024] Preferably, the method for preparing the active material includes any of the following methods:

[0025] S1: Mix the first metal powder and the second metal powder to obtain a mixed metal powder;

[0026] S2: Place the mixed metal powder in a jacket and evacuate it, and perform hot isostatic pressing at 1200°C - 1450°C to obtain a metal alloy material;

[0027] S3: Perform hot hydrogen treatment on the metal alloy material in a hydrogen atmosphere at 500 - 800°C to obtain the active material;

[0028] Or,

[0029] S1: Mix the first metal powder and the second metal powder to obtain a mixed metal powder;

[0030] S2: Granulate the mixed metal powder, and then press the obtained mixed metal powder to obtain a green compact;

[0031] S3: Perform vacuum sintering treatment on the green compact at 1200°C - 1450°C to obtain a metal alloy material;

[0032] S4: Perform hot hydrogen treatment on the metal alloy material in a hydrogen atmosphere at 500 - 800°C to obtain the active material.

[0033] In a second aspect, the present invention provides an active material prepared by the method for preparing the active material described above.

[0034] The active material and its preparation method provided by the present invention can achieve controllability of density and mechanical properties within a certain range through composition design of the active material; and the active material has sufficient mechanical properties under high-speed impact conditions to ensure integrity, and can also provide sufficient additional chemical energy to improve the post-damage effect of fragments. The present invention uses hot hydrogen treatment to hydrogenate the fragments, which can not only regulate the mechanical properties of the active fragments, but also improve the explosion damage performance of the active fragments; at the same time, the preparation method has a short process flow, high efficiency, and controllable density and mechanical properties. Description of the Drawings

[0035] To more clearly illustrate the technical solutions in the present invention or the prior art, the following will briefly introduce the drawings required for the description of the embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0036] Figure 1 It is a schematic diagram of the preparation process of the active material in Embodiment 1 provided by the present invention.

[0037] Figure 2 It is the physical object of the hydrogen-permeated fragment obtained in Embodiment 1 provided by the present invention.

[0038] Figure 3 It is a schematic diagram of the preparation process of the active material in Embodiment 2 provided by the present invention. Detailed implementation manners

[0039] To make the objectives, technical solutions, and advantages of the present invention clearer, the following will clearly and completely describe the technical solutions in the present invention in conjunction with the drawings in the present invention. Obviously, the described embodiments are some embodiments of the present invention, rather than all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope protected by the present invention.

[0040] Unless otherwise specified, all kinds of raw materials used in the examples and comparative examples are commercially available conventional raw materials, and the technical means used are conventional means well-known to those skilled in the art.

[0041] Embodiment 1

[0042] This embodiment provides an active material with high energy release, and its preparation method includes the following steps (for the schematic diagram of the process, see Figure 1 )

[0043] (1) Prepare the active raw material powder by mechanical mixing method. 4.8 kg of pure titanium powder with a particle size of 10 - 60 μm, 18 kg of tantalum powder with a particle size of 10 - 60 μm, and 1.2 kg of tungsten powder with a particle size of 3 - 20 μm are placed in a mixer and mixed thoroughly for 120 min to mix the raw material powder evenly. Weigh 100 g of the raw material powder and measure its tapped density.

[0044] (2) Place a certain amount of the raw material powder obtained in step (1) into a steel jacket with a specific volume according to the tapped density, and use vibration to assist powder loading during the process. After powder loading, the air in the jacket is pumped out and the jacket is sealed. Subsequently, the jacket is subjected to hot isostatic pressing at 1350 °C and 145 MPa for 140 min.

[0045] (3)The billet after hot isostatic pressing removes the outer sheath, grinds to remove the wire cutting marks, and uses alcohol or acetone to remove the surface oil stain.

[0046] (4)Place the billet obtained in step (3) in a tube furnace, evacuate the air in the furnace with argon, after evacuation, introduce hydrogen, raise the furnace temperature to 600 °C and keep it warm for 120 min, the hydrogen flow rate is 1 - 2 L / min, the billet is cooled with the furnace after treatment, and the tail gas needs to be ignited for treatment.

[0047] (5)Process the billet obtained in step (4) into a specific size and shape according to requirements. See the physical drawing in Figure 2 .

[0048] Example 2

[0049] This example provides a high-energy release active material, and the difference in its preparation method from that of Example 1 is only that: in step (2), the pressure of hot isostatic pressing is 170 MPa and the temperature is 1500 °C.

[0050] Example 3

[0051] This example provides a high-energy release active material, and its preparation method includes the following steps (see the process schematic diagram in Figure 3 ):

[0052] (1)Prepare the active raw material powder by mechanical mixing method. Put 4.8 kg of pure titanium powder with a particle size of 10 - 60 μm, 14.4 kg of tantalum powder with a particle size of 10 - 60 μm, and 4.8 kg of tungsten powder with a particle size of 3 - 20 μm into a mixer and mix them evenly for 120 min.

[0053] (2)Granulate and screen the raw material powder obtained in step (1) to obtain a powder with better fluidity.

[0054] (3)The powder obtained in step (2) is pressed into shape by a powder metallurgy forming press with a pressure of 35 MPa to obtain a green compact with a specified shape.

[0055] (4)Place the green compact obtained in step (3) in a vacuum sintering furnace at 1200 °C - 1500 °C and sinter for 120 min - 160 min.

[0056] (5)Place the billet obtained in step (4) in a tube furnace, evacuate the air in the furnace with argon, after evacuation, introduce hydrogen, raise the furnace temperature to 500 °C and keep it warm for 90 min, the hydrogen flow rate is 1 - 2 L / min, the billet is cooled with the furnace after treatment, and the tail gas needs to be ignited for treatment.

[0057] (6)Screen the sample obtained in step (5) to obtain qualified fragments.

[0058] Example 4

[0059] This embodiment provides an active material with high energy release. The difference in its preparation method from that of Embodiment 1 is only that: the raw material powder includes: 2.4 kg of pure titanium powder with a particle size of 10 - 60 μm, 14.4 kg of tantalum powder with a particle size of 10 - 60 μm, and 7.2 kg of tungsten powder with a particle size of 3 - 20 μm.

[0060] Embodiment 5

[0061] This embodiment provides an active material with high energy release. The difference in its preparation method from that of Embodiment 1 is only that: the titanium powder is replaced with TA15 powder of the same specification in equal amount, and the remaining steps are the same as those in Embodiment 1.

[0062] Embodiment 6

[0063] This comparative example provides an active material with high energy release. The difference in its preparation method from that of Embodiment 1 is only that: the titanium powder is replaced with TC4 powder of the same specification in equal amount, and the remaining steps are the same as those in Embodiment 1.

[0064] Comparative Example 1

[0065] This comparative example provides an active material with high energy release. The difference in its preparation method from that of Embodiment 1 is only that: step (4) is not included, and after hot isostatic pressing, it is directly machined into fragments of a specific shape.

[0066] Comparative Example 2

[0067] This comparative example provides an active material with high energy release. The difference in its preparation method from that of Embodiment 1 is only that: the titanium powder is replaced with zirconium powder of the same specification in equal amount, and the remaining steps are the same as those in Embodiment 1.

[0068] Test Example

[0069] The present invention tests the density, energy release, etc. of the fragments in the above embodiments and comparative examples, and the test results are shown in Table 1.

[0070] The test methods include:

[0071] Density test method for fragments: According to "GB / T 3850 - 2015 Test Method for Density of Dense Sintered Metal Materials and Cemented Carbides", the density of the fragments is tested 5 times and the average value is taken.

[0072] Combustion heat test method: 0.5 g of the active material sample is put into an oxygen bomb, and a combustion reaction is carried out under high-pressure oxygen conditions. The heat released during the reaction is measured by a calorimeter, and the calorific value of the fragment is calculated.

[0073] Fracture strain test method: Conduct 5 tests in accordance with "GB / T 7314-2017 Metallic materials - Compression test at room temperature", record the engineering strain values at which the material cracks and fails, and take the average value.

[0074] Compressive strength test method: Conduct 5 tests in accordance with "GB / T 7314-2017 Metallic materials - Compression test at room temperature", record the maximum engineering stress values before the material cracks and fails, and take the average value.

[0075] Hydrogen content test method: Use a balance with a precision of 0.0001 g to measure the masses of the samples before and after hot hydrogen treatment, which are m1 and m2 respectively. The hydrogen content is 100%×(m2 - m1) / m2.

[0076] Table 1

[0077]

[0078] For the active material with a hydrogen content of 0.5 - 0.6%, compared with the hydrogen-free material, its energy release can be increased by about 5.5%. At the same time, the introduction of hydrogen elements can also optimize the mechanical properties of the material. This increase in energy release and the improvement of mechanical properties together enhance the damage aftereffect of the active fragment.

[0079] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features; and these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing an active material, characterized in that: include: S1: mixing a first metal powder and a second metal powder to obtain a mixed metal powder; S2: pressing the mixed metal powder, and then performing vacuum sintering to obtain a metal alloy material; S3: subjecting the metal alloy material to thermal hydrogen treatment to obtain the active material; The first metal powder is a mixture of titanium-containing powder and pure tantalum powder, and the titanium-containing powder is pure titanium powder and / or titanium alloy powder; The density of the second metal powder is 15-19.5 g / cm³, and the second metal powder includes pure tungsten powder.

2. The method for preparing the active material according to claim 1, characterized in that: The titanium alloy powder includes TA15 powder and / or TC4 powder.

3. The method for preparing the active material according to claim 1 or 2, characterized in that: The mass ratio of the first metal powder to the second metal powder is (4-99):

1.

4. The method for preparing the active material according to claim 1 or 2, characterized in that: The first metal powder is composed of titanium-containing powder and pure tantalum powder in a mass ratio of 1: (1.8-8.9).

5. The method for preparing the active material according to claim 1 or 2, characterized in that: The particle size of the first metal powder is 10-80 μm; the particle size of the second metal powder is 3-20 μm.

6. The method for preparing the active material according to claim 1 or 2, characterized in that: S3 includes subjecting the metal alloy material to a thermal hydrogen treatment in a hydrogen atmosphere at 500-800°C.

7. The method for preparing the active material according to claim 6, characterized in that: In S3, the flow rate of hydrogen is 0.5~3L / min.

8. The method for preparing the active material according to claim 1 or 2, characterized in that: In S2, the vacuum sintering treatment conditions include: sintering at 1200° C. to 1500° C. for 120 min to 180 min.

9. A method for preparing an active material, characterized in that: The preparation method of the active material includes any one of the following: S1: mixing a first metal powder and a second metal powder to obtain a mixed metal powder; the first metal powder is a mixture of titanium-containing powder and pure tantalum powder, the titanium-containing powder is pure titanium powder and / or titanium alloy powder; the density of the second metal powder is 15-19.5 g / cm³, and the second metal powder includes pure tungsten powder; S2: placing the mixed metal powder in a bag and evacuating the bag, and performing hot isostatic pressing at 1200° C. to 1450° C. to obtain a metal alloy material; S3: subjecting the metal alloy material to a thermal hydrogen treatment in a hydrogen atmosphere at 500-800° C. to obtain the active material; or, S1: mixing a first metal powder and a second metal powder to obtain a mixed metal powder; the first metal powder is a mixture of titanium-containing powder and pure tantalum powder, the titanium-containing powder is pure titanium powder and / or titanium alloy powder; the density of the second metal powder is 15-19.5 g / cm³, and the second metal powder includes pure tungsten powder; S2: granulating the mixed metal powder, and then pressing the obtained mixed metal powder to obtain a compact; S3: performing vacuum sintering treatment on the compact at 1200° C. to 1450° C. to obtain a metal alloy material; S4: subjecting the metal alloy material to a thermal hydrogen treatment in a hydrogen atmosphere at 500-800° C. to obtain the active material.

10. An active material, characterized in that The active material is prepared by the preparation method of any one of claims 1 to 9.

Images