阅读说明：本技术 一种碳化硼轻质防弹材料及其制备方法 (Boron carbide light bulletproof material and preparation method thereof ) 是由 汪兆栋 陈猛 徐罗俊 周高杰 杨婷 刘志诚 于 2021-10-12 设计创作，主要内容包括：本发明涉及一种碳化硼轻质防弹材料,所述防弹材料按重量比,由碳化硼粉末80-95%、二氧化钛粉3-8%,炭黑粉1-5%、碳化硅粉1-5%,氧化石墨烯粉0.5％～3％,二硅化钼粉0.02-0.1%组成,所述防弹材料选择适宜的原材料进行搭配,经特殊工艺制备得到性能强,密度低,成本低的新型轻质材料,并适用于大规模工业化生产。(The invention relates to a boron carbide light bulletproof material, which consists of 80-95% of boron carbide powder, 3-8% of titanium dioxide powder, 1-5% of carbon black powder, 1-5% of silicon carbide powder, 0.5-3% of graphene oxide powder and 0.02-0.1% of molybdenum disilicide powder by weight ratio, and the bulletproof material is prepared by matching proper raw materials through a special process to obtain a novel light material with strong performance, low density and low cost, and is suitable for large-scale industrial production.)

1. The boron carbide light bulletproof material is characterized by comprising, by weight, 80-95% of boron carbide powder, 3-8% of titanium dioxide powder, 1-5% of carbon black powder, 1-5% of silicon carbide powder, 0.5-3% of graphene oxide powder and 0.02-0.1% of molybdenum disilicide powder.

2. The boron carbide lightweight ballistic resistant material of claim 1 wherein the average particle size of the graphene oxide powder and the molybdenum disilicide powder are each 0.5 to 5 microns.

3. The boron carbide lightweight ballistic resistant material of claim 1 wherein the average particle size of the boron carbide powder is 0.5-5 microns and the average particle size of the titanium dioxide powder, carbon black powder and silicon carbide powder is 0.1-0.5 microns.

4. The boron carbide lightweight ballistic material of claim 1, wherein the method of making the ballistic material comprises the steps of:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 1.5-3h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1-1.5h again, and then passing through a 120-mesh screen to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, and pressing to obtain a biscuit;

(4) and (3) placing the biscuit in a sintering furnace, heating to 2015-heat-insulated 2200 ℃ for sintering under the protection of argon, preserving heat for 1.5-3h, cooling, grinding and polishing to obtain the bulletproof material.

5. The method for preparing the boron carbide lightweight bulletproof material of claim 4, wherein: the biscuit is pressed and molded under the pressure of 110-120MPa, and the pressure maintaining time is 10-20 s.

6. The method for preparing the boron carbide lightweight bulletproof material of claim 4, wherein: the sintering furnace is a vacuum hot pressing furnace.

7. The method for preparing the boron carbide lightweight bulletproof material of claim 4, wherein: the temperature rise refers to the process of starting pressurization from 1200 ℃, the pressurization pressure is 20-40MPa, the temperature is raised to 1700-DEG C1900 ℃ at 30-50 ℃/min, the temperature is preserved for 0.5h, and then the temperature is raised to 2015-DEG C2200 ℃ at 20-30 ℃/min.

Technical Field

The invention belongs to the technical field of material synthesis, and particularly relates to a boron carbide light bulletproof material and a preparation method thereof.

Background

Boron carbide has a series of excellent performances such as high melting point, high hardness, low density, good thermal stability, strong chemical erosion resistance, good neutron absorption capacity and the like, is widely applied to the fields of energy and military, is a raw material of the most common bulletproof material, has extraordinary hardness (35-45 Gpa), and has nearly constant high-temperature hardness which is incomparable with other materials. The ceramic material made of boron carbide has better bulletproof performance and is also an ideal armor material.

The preparation process of the boron carbide ceramic is roughly divided into the processes of powder preparation, forming, sintering, subsequent processing and the like, wherein the powder forming process and the sintering method are very critical steps and have great influence on the final performance of a finished product. Therefore, it is crucial to select the raw materials of the ballistic material reasonably and to select the appropriate shaping and sintering method.

In order to obtain a bulletproof material with good performance, good quality and low cost, the three factors need to be balanced so as to lower the density and the cost on the premise of meeting the bulletproof performance, therefore, the invention provides a novel light high-performance boron carbide bulletproof material, which better meets the market requirement.

Disclosure of Invention

The invention aims to provide a boron carbide light bulletproof material and a preparation method thereof, wherein the bulletproof material is prepared by matching proper raw materials through a special process, and is a novel light material with strong performance, low density and low cost, and is suitable for large-scale industrial production.

The invention provides a boron carbide light bulletproof material, which comprises, by weight, 80-95% of boron carbide powder, 3-8% of titanium dioxide powder, 1-5% of carbon black powder, 1-5% of silicon carbide powder, 0.5-3% of graphene oxide powder and 0.02-0.1% of molybdenum disilicide powder.

In the above boron carbide lightweight bulletproof material, it is preferable that the average particle diameters of the graphene oxide powder and the molybdenum disilicide powder are both 0.5 to 5 μm.

In the above-mentioned boron carbide lightweight bulletproof material, preferably, the average particle size of the boron carbide powder is 0.5 to 5 micrometers, and the average particle sizes of the titanium dioxide powder, the carbon black powder and the silicon carbide powder are all 0.1 to 0.5 micrometers.

The invention also provides a preparation method of the boron carbide light bulletproof material, which comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 1.5-3h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1-1.5h again, and then passing through a 120-mesh screen to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, and pressing to obtain a biscuit;

(4) and (3) placing the biscuit in a sintering furnace, heating to 2015-heat-insulated 2200 ℃ for sintering under the protection of argon, preserving heat for 1.5-3h, cooling, grinding and polishing to obtain the bulletproof material.

In the preparation method of the boron carbide lightweight bulletproof material, the biscuit is preferably pressed and molded under the pressure of 110-120MPa, and the pressure holding time is 10-20 s.

In the above method for preparing a lightweight boron carbide bulletproof material, preferably, the sintering furnace is a vacuum hot-pressing furnace.

In the preparation method of the boron carbide light bulletproof material, preferably, the temperature rise means that the pressurization is started from 1200 ℃, the pressurization pressure is 20-40MPa, the temperature rise is carried out at 30-50 ℃/min to 1700-1900 ℃, the temperature is kept for 0.5h, and then the temperature rise is carried out at 20-30 ℃/min to 2015-2200 ℃.

According to the invention, boron carbide with high hardness and low density is used as a basic raw material, titanium dioxide powder, carbon black powder and silicon carbide powder are combined, graphene oxide is added, the strength and toughness of the bulletproof material are improved, molybdenum disilicide is added, the hardness and oxidation resistance are enhanced, meanwhile, the dispersibility of graphene oxide powder is improved, and agglomeration is avoided. And the machining method is simple and suitable for large-scale application.

Detailed Description

The technical solution of the present invention is further described in detail by the following embodiments.

Example 1

Raw materials: 91.25% of boron carbide powder, 4.8% of titanium dioxide powder, 1.2% of carbon black powder, 1.5% of silicon carbide powder, 1.2% of graphene oxide powder and 0.05% of molybdenum disilicide powder.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 3 hours by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1 hour again, and then sieving through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 20s, and pressing to obtain a biscuit;

(4) placing the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, keeping the pressure at 30MPa, heating to 1800 ℃ at 35 ℃/min, keeping the temperature for 0.5h, then heating to 2200 ℃ at 25 ℃/min, sintering, keeping the temperature for 2.5h, cooling, grinding and polishing to obtain the bulletproof material.

Example 2

Raw materials: 83.42% of boron carbide powder, 7.9% of titanium dioxide powder, 2.6% of carbon black powder, 3.6% of silicon carbide powder, 2.4% of graphene oxide powder and 0.08% of molybdenum disilicide powder.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1.5h again, and then sieving the mixture through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) placing the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, keeping the pressure at 35MPa, heating to 1900 ℃ at 50 ℃/min, keeping the temperature for 0.5h, then heating to 2105 ℃ at 20 ℃/min, sintering, keeping the temperature for 3h, cooling, grinding, and polishing to obtain the bulletproof material.

Example 3

Raw materials: according to the weight ratio, the boron carbide powder is 86.84%, the titanium dioxide powder is 5.4%, the carbon black powder is 3.8%, the silicon carbide powder is 2.1%, the graphene oxide powder is 1.8%, and the molybdenum disilicide powder is 0.06%.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2 hours by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1 hour again, and then sieving through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 115MPa, keeping the pressure for 10s, and pressing to obtain a biscuit;

(4) placing the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, keeping the pressure at 20MPa, heating to 1700 ℃ at 30 ℃/min, keeping the temperature for 0.5h, then heating to 2105 ℃ at 30 ℃/min, sintering, keeping the temperature for 1.5h, cooling, grinding and polishing to obtain the bulletproof material.

Example 4

Raw materials: 83.42% of boron carbide powder, 7.9% of titanium dioxide powder, 2.6% of carbon black powder, 3.6% of silicon carbide powder, 2.4% of graphene oxide powder and 0.08% of molybdenum disilicide powder.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1.5h again, and then sieving the mixture through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

Example 5

Raw materials: 83.42% of boron carbide powder, 7.9% of titanium dioxide powder, 2.6% of carbon black powder, 3.6% of silicon carbide powder, 2.4% of graphene oxide powder and 0.08% of molybdenum disilicide powder.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder, silicon carbide powder, graphene oxide powder and molybdenum disilicide into a ball mill, wet-milling for 2.8 hours by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) spray drying and granulating the obtained slurry to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

Comparative example 1

Raw materials: according to the weight ratio, the boron carbide powder accounts for 85.9 percent, the titanium dioxide powder accounts for 7.9 percent, the carbon black powder accounts for 2.6 percent, and the silicon carbide powder accounts for 3.6 percent.

Wherein, the average grain diameter of the boron carbide powder is 1.25um, the average grain diameter of the titanium dioxide powder is 0.24um, the average grain diameter of the carbon black powder is 0.35um, and the average grain diameter of the silicon carbide powder is 0.16 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) spray drying and granulating the obtained slurry to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

Comparative example 2

Raw materials: according to the weight ratio, the boron carbide powder is 83.5%, the titanium dioxide powder is 7.9%, the carbon black powder is 2.6%, the silicon carbide powder is 3.6%, and the graphene oxide powder is 2.4%.

Wherein the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, and the average particle size of graphene oxide powder is 2.48 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder into the slurry according to the parts by weight, performing ball milling for 1.5h again, and then sieving through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

Comparative example 3

Raw materials: according to the weight ratio, the boron carbide powder is 85.82 percent, the titanium dioxide powder is 7.9 percent, the carbon black powder is 2.6 percent, the silicon carbide powder is 3.6 percent, and the molybdenum disilicide powder is 0.08 percent.

Wherein, the average grain diameter of the boron carbide powder is 1.25um, the average grain diameter of the titanium dioxide powder is 0.24um, the average grain diameter of the carbon black powder is 0.35um, the average grain diameter of the silicon carbide powder is 0.16um, and the average grain diameter of the molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1.5h again, and then sieving the mixture through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

Comparative example 4

Raw materials: 81.02% of boron carbide powder, 7.9% of titanium dioxide powder, 2.6% of carbon black powder, 3.6% of silicon carbide powder, 4.8% of graphene oxide powder and 0.08% of molybdenum disilicide powder.

Wherein, the average particle size of boron carbide powder is 1.25um, the average particle size of titanium dioxide powder is 0.24um, the average particle size of carbon black powder is 0.35um, the average particle size of silicon carbide powder is 0.16um, the average particle size of graphene oxide powder is 2.48um, and the average particle size of molybdenum disilicide powder is 1.36 um.

The preparation method comprises the following steps:

(1) according to the weight parts, placing boron carbide powder, titanium dioxide powder, carbon black powder and silicon carbide powder in a ball mill, wet-milling for 2.8h by taking deionized water as a medium, and then sieving by a 120-mesh sieve to obtain slurry;

(2) adding graphene oxide powder and molybdenum disilicide powder into the slurry according to the parts by weight, performing ball milling for 1.5h again, and then sieving the mixture through a 120-mesh sieve to obtain slurry, and performing spray drying granulation to obtain granules;

(3) placing the granulated material in a mould, pressing and forming under the pressure of 110MPa, keeping the pressure for 15s, and pressing to obtain a biscuit;

(4) and putting the biscuit in a vacuum hot pressing furnace, pressurizing from 1200 ℃ under the protection of argon, wherein the pressurizing pressure is 35MPa, heating to 2105 ℃ at 30 ℃/min, sintering, preserving heat for 3h, cooling, grinding and polishing to obtain the bulletproof material.

The samples prepared in the test examples are subjected to performance detection tests, wherein the density of the samples is determined according to the method for determining QB/T1010-2015 ceramic material and pigment true density; the bending strength adopts a GB/T4741-1999 ceramic material bending strength test method; fracture toughness adopts a GB/T23806-2009 fine ceramic fracture toughness test method unilateral pre-crack beam (SEPB) method; the microhardness adopts the Vickers hardness test method of GB/T16534 and 1996 engineering ceramics. The results are as follows:

the test example results show that, compared with comparative examples 1 and 2, when a proper amount of graphene oxide is added in the formula, the bending strength and the fracture toughness can be improved, and the microhardness is improved. Comparative examples 2, 4 and 5 show that batch secondary grinding and programmed sintering have a significant effect on the reduction of the sample density and the improvement of the fracture toughness under the same formulation.

In conclusion, the bulletproof material with lighter weight and strong protection performance can be prepared by the formula and the preparation method. And the preparation process is simple and is beneficial to industrial application.