CN115073145A - Aluminum oxide bulletproof ceramic and preparation method thereof - Google Patents

Aluminum oxide bulletproof ceramic and preparation method thereof Download PDF

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CN115073145A
CN115073145A CN202110275683.1A CN202110275683A CN115073145A CN 115073145 A CN115073145 A CN 115073145A CN 202110275683 A CN202110275683 A CN 202110275683A CN 115073145 A CN115073145 A CN 115073145A
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temperature
stage
alumina
oxide
ceramic
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黄超
冯金环
黄迎峰
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Shanghai Zhaoming Industrial Co ltd
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Shanghai Zhaoming Industrial Co ltd
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Abstract

The invention relates to the technical field of composite ceramic preparation, in particular to pressureless sintering boron carbide bulletproof ceramic and a preparation method thereof; an alumina bulletproof ceramic comprises the following components in parts by weight: 99-99.5 parts of alumina and 0.5-1 part of assistant; the invention adopts a low-temperature slow burning process, inhibits the growth of crystals in the conversion process, and improves the density and the performance of the ceramic; the specifications of the bulletproof ceramic can be diversified, the bulletproof ceramic can have radian, and the bulletproof ceramic can be more attached to a human body after being spliced into an arc shape, so that a larger gap can not be caused, and the bulletproof performance can be further improved; the alumina bulletproof ceramic prepared by the invention has good sintering performance, stable product size, high strength and lighter weight; the alumina bulletproof ceramic has excellent bulletproof performance, lighter weight and relatively low price, so that the alumina bulletproof ceramic becomes the most widely used bulletproof material at present and is in the leading position in the domestic ceramic plugboard market.

Description

Aluminum oxide bulletproof ceramic and preparation method thereof
Technical Field
The invention relates to the technical field of composite ceramic preparation, in particular to an alumina bulletproof ceramic and a preparation method thereof
Background
From the historical development of bulletproof armor materials, the bulletproof armor is developed towards light weight, high efficiency and low price from the original traditional metal materials (aluminum and steel) to the advanced ceramic materials and composite materials. The steel plate is the material which is applied to the hard bulletproof clothes at the earliest, the protection level of the soft bulletproof clothes is greatly improved, but the protection capability is limited, and only the protection can be realizedThe attack of the lead core bullet and the common steel core bullet is resisted, and the defects of high weight, easy bouncing and the like are overcome; al (Al) 2 O 3 Compared with a steel plate, the ceramic material is further improved, the hardness directly determines the anti-elasticity performance of the core protection inserting plate, the density directly determines the weight of the core protection inserting plate, the weight is light, the density is less than 1/2 of the steel plate, the hardness is high, the better anti-elasticity performance is achieved, and the bouncing phenomenon is avoided.
However, the currently prepared alumina bulletproof ceramic has high strength, smooth surface, no air holes inside and stable dimensional tolerance range, and needs to be optimized in material and process to prepare alumina bulletproof ceramic with excellent performance.
Disclosure of Invention
In order to solve the above problems, a first aspect of the present invention provides an alumina bulletproof ceramic, comprising the following components in parts by weight: 99 to 99.5 portions of alumina and 0.5 to 1 portion of auxiliary agent.
Preferably, the crystalline form of alumina is the alpha form.
Preferably, the particle size of the alumina is 0.5-0.8 um.
Preferably, the adjuvant is an oxide.
Preferably, the oxide is selected from one or more of zinc oxide, magnesium oxide, aluminum oxide, calcium oxide, silicon oxide, potassium oxide, sodium oxide, yttrium oxide, zirconium dioxide.
Preferably, the oxide is a mixture of yttrium oxide, zirconium dioxide, magnesium oxide.
Preferably, the weight ratio of the yttrium oxide to the zirconium dioxide to the magnesium oxide is (8-12): (7-12): 1.
Preferably, the weight ratio of the yttrium oxide to the zirconium dioxide to the magnesium oxide is (9-11): (8-10): 1.
The second aspect of the invention provides a preparation method of an alumina bulletproof ceramic, which comprises the following steps:
(1) adding 99-99.5 parts of alumina and 0.5-1 part of auxiliary agent into a ball mill for ball milling and mixing for 18-30 h;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the feeding pressure is 40-60MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 150-1500 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 0.5-5cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
Preferably, the temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 h; in the second stage, the temperature is raised from 300 ℃ to 500-600 ℃, and the temperature rise time is 6 h; in the third stage, the temperature is raised from 500-1100 ℃ to 1000-1100 ℃ for 8 h; in the fourth stage, the temperature is increased from 1100 ℃ at 1000-; in the fifth stage, the temperature is increased from 1300 ℃ to 1400 ℃ to 1450 ℃ to 1500 ℃ for 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1500 ℃ to 1550 ℃ to 1650 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is preserved for 4h at 1550-; in the eighth stage, the temperature is reduced from 1550-; stopping heating natural gas in the ninth stage, and cooling from 1300-1400 ℃ to 800-900 ℃; and in the tenth stage, stopping blowing by the blower, and naturally cooling to room temperature from 800-900 ℃.
Further, the temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
Advantageous effects
1. The alumina bulletproof ceramic prepared by the invention has good sintering performance, stable product size, high strength and lighter weight.
2. The alumina bulletproof ceramic has excellent bulletproof performance, lighter weight and relatively low price, so that the alumina bulletproof ceramic becomes the most widely used bulletproof material at present and is dominant in the domestic ceramic insert plate market.
3. The invention adopts a low-temperature slow burning process, inhibits the growth of crystals in the conversion process and improves the density and the performance of the ceramic.
4. The specification of the bulletproof ceramic can be diversified, the bulletproof ceramic can have radian, and the bulletproof ceramic can be more attached to a human body after being spliced into an arc shape, so that a larger gap can not be caused, and the bulletproof performance can be more improved.
Detailed Description
The technical features of the technical solutions provided by the present invention are further clearly and completely described below with reference to the specific embodiments, and the scope of protection is not limited thereto.
The words "preferred", "more preferred", and the like, in the present invention refer to embodiments of the invention that may provide certain benefits, under certain circumstances. However, other embodiments may be preferred, under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range describing features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to encompass any and all subranges subsumed therein. For example, a stated range from "1 to 10" should be considered to include any and all subranges between the minimum value of 1 and the maximum value of 10. Exemplary subranges of the range 1 to 10 include, but are not limited to, 1 to 6.1, 3.5 to 7.8, 5.5 to 10, and the like.
In order to solve the above problems, a first aspect of the present invention provides an alumina bulletproof ceramic, comprising the following components in parts by weight: 99 to 99.5 portions of alumina and 0.5 to 1 portion of auxiliary agent.
In a preferred embodiment, the crystalline form of alumina is the alpha form.
In a preferred embodiment, the alumina has a particle size of 0.5 to 0.8 um.
In a preferred embodiment, the alumina is selected from Shanghai Bingming industries, Inc. with a VITAL alumina granulation powder specification.
In a preferred embodiment, the adjuvant is an oxide.
In a preferred embodiment, the oxide is selected from one or more of zinc oxide, magnesium oxide, aluminum oxide, calcium oxide, silicon oxide, potassium oxide, sodium oxide, yttrium oxide, zirconium dioxide.
In a more preferred embodiment, the oxide is a mixture of yttria, zirconia, magnesia.
In a preferred embodiment, the weight ratio of the yttrium oxide, the zirconium dioxide and the magnesium oxide is (8-12): (7-12): 1.
In a preferred embodiment, the weight ratio of the yttrium oxide, the zirconium dioxide and the magnesium oxide is (9-11): (8-10): 1.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu-Shu-Xuanling biological technology Limited company, and the mass content is 99.9 percent.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
In experiments, the yttrium oxide, the zirconium dioxide, the magnesium oxide and the alumina particles form an interaction system during sintering, the alumina can be sintered at low temperature, the strength of the prepared ceramic is high, and the finer the alumina particles are, the stronger the interaction between the alumina particles and the auxiliary agent is, and the higher the strength of the prepared ceramic is; when the content of the magnesium oxide in the system is low, the recrystallization phenomenon in the sintering process can be restrained, and the strength of the alumina ceramic is improved; however, the addition amount of magnesium oxide is too large, which hinders the interaction between systems, and raises the sintering temperature, and alumina ceramics having high strength cannot be produced at a low temperature.
The second aspect of the invention provides a preparation method of an alumina bulletproof ceramic, which comprises the following steps:
(1) adding 99-99.5 parts of alumina and 0.5-1 part of auxiliary agent into a ball mill for ball milling and mixing for 18-30 h;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the feeding pressure is 40-60MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 150-1500 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 0.5-5cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
In a preferred embodiment, the temperature and the heating time of the ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 h; in the second stage, the temperature is raised from 300 ℃ to 500-600 ℃, and the temperature rise time is 6 h; in the third stage, the temperature is raised from 500-1100 ℃ to 1000-1100 ℃ for 8 h; in the fourth stage, the temperature is increased from 1100 ℃ at 1000-; in the fifth stage, the temperature is increased from 1300 ℃ to 1400 ℃ to 1450 ℃ to 1500 ℃ for 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1500 ℃ to 1550 ℃ to 1650 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is preserved for 4h at 1550-; in the eighth stage, the temperature is reduced from 1550-; stopping heating natural gas in the ninth stage, and cooling from 1300-1400 ℃ to 800-900 ℃; and in the tenth stage, stopping blowing by the blower, and naturally cooling to room temperature from 800-900 ℃.
In a more preferable embodiment, the temperature and the heating time of the ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 h; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
In the experimental process, the temperature rise and the heat preservation time are prolonged, the volume density of the ceramic is continuously improved, and the strength is improved; when the sintering temperature is not high, the sintering can be carried out for a longer holding time, the sintering temperature is too high, or the holding time is too long at the sintering temperature, the excessive sintering phenomena such as coarse crystal grains, density reduction and the like can be caused, and the strength of the ceramic is reduced.
Example 1
An alumina bulletproof ceramic comprises the following components in parts by weight: 99 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.44 part of zirconium dioxide and 0.06 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.44 part of zirconium dioxide and 0.06 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is raised from 300 ℃ to 600 ℃, and the temperature raising time is 6 h; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 2
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.5 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.46 part of zirconium dioxide and 0.04 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.5 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.46 part of zirconium dioxide and 0.04 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 3
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric pushed slab kiln, keeping 2cm gap arrangement among the green bodies, controlling the temperature rise time and speed of ten stages of the electric pushed slab kiln, sintering and cooling to obtain the alumina bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling to 900 ℃ from 1300 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Bingming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 4
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai summon industries, Inc., and the particle size of the alumina is 1.2-1.5 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 5
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.1 part of zirconium dioxide and 0.2 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.1 part of zirconium dioxide and 0.2 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 6
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, the heating rate is 10 ℃/min, and the heating and heat preservation time is 5 h; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, the temperature increase rate is 10 ℃/min, and the temperature increase and preservation time is 6 h; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃, the temperature raising rate is 10 ℃/min, and the temperature raising and preserving time is 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, the temperature increase rate is 10 ℃/min, and the temperature increase and preservation time is 6 h; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, the temperature increasing rate is 10 ℃/min, and the temperature increasing and preserving time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, the temperature increase rate is 10 ℃/min, and the temperature increase and preservation time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, the temperature rise and reduction rate is 10 ℃/min, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu-Shu-Xuanling biological technology Limited company, and the mass content is 99.9 percent.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 7
An alumina bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1525 ℃ for 6 h; in the seventh stage, the heat preservation time is 4h from 1525 ℃; in the eighth stage, the temperature is reduced from 1525 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Example 8
The aluminum oxide bulletproof ceramic comprises the following components in parts by weight: 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide.
A preparation method of an alumina bulletproof ceramic comprises the following steps:
(1) adding 99.2 parts of aluminum oxide, 0.5 part of yttrium oxide, 0.45 part of zirconium dioxide and 0.05 part of magnesium oxide into a ball mill for ball milling and mixing for 24 hours;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 30HZ, the air inlet temperature is 265 ℃, the air outlet temperature is 1100 ℃, and the feeding pressure is 52MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 300 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 2cm of gap arrangement among the green bodies, controlling the heating time and speed of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
The temperature and the heating time of ten stages of the electric pushing plate kiln in the step (4) are increased from room temperature to 300 ℃ in the first stage, and the heating time is 5 hours; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 10 h; in the seventh stage, the temperature is kept at 1630 ℃ for 10 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
The alumina is selected from Shanghai Suming industry Co., Ltd, and is VITAL alumina granulation powder, and the particle size of the alumina is 0.5-0.8 um.
The yttrium oxide purchasing manufacturer is Shandong Liang New Material science and technology company, and the specification model is LA-10.
The zirconium dioxide purchasing manufacturer is Hubei Chu scintillation biotechnology limited company, and the mass content is 99.9%.
The magnesium oxide purchasing manufacturer is Hangzhou Hengnan New Material Co., Ltd, and the specification is HN-Mg 50.
Performance testing
1. Testing of sintering density: the sintered density of the sample was measured using a densitometer using archimedes' principle.
2. And (3) testing the bending strength: the three-point bending strength was measured in an INSTRON-5566 universal material testing machine using digital display bending strength, with a test specimen specification of 3mm x 4mm x 36mm, span of 20mm, and loading speed of 0.5 mm/min.
3. Vickers hardness test: the vickers hardness of the test specimen was measured using a digital vickers hardness tester.
The alumina ballistic resistant ceramics prepared in examples 1-8 were tested for performance using the test methods described above and the test data is shown in table 1.
Examples Density) (g/cm 3 ) Bending strength (Mpa) Vickers hardness (GPa)
Example 1 3.9 358 16.9
Example 2 3.91 367 17.1
Example 3 3.93 375 17.4
Example 4 3.89 349 16.4
Example 5 3.88 342 15.9
Examples6 3.85 337 15.3
Example 7 3.82 332 15.1
Example 8 3.8 329 14.8
TABLE 1

Claims (10)

1. The aluminum oxide bulletproof ceramic is characterized by comprising the following components in parts by weight: 99 to 99.5 portions of alumina and 0.5 to 1 portion of auxiliary agent.
2. The alumina ballistic resistant ceramic of claim 1 wherein the crystalline form of alumina is the alpha form.
3. The alumina ballistic resistant ceramic of claim 1 wherein the alumina has a particle size of 0.5 to 0.8 um.
4. The alumina ballistic resistant ceramic of claim 1 wherein the adjunct is an oxide.
5. The alumina ballistic resistant ceramic according to claim 4 wherein the oxide is selected from one or more of zinc oxide, magnesium oxide, aluminum oxide, calcium oxide, silicon oxide, potassium oxide, sodium oxide, yttrium oxide, zirconium dioxide.
6. The alumina ballistic resistant ceramic of claim 5 wherein the oxide is a mixture of yttria, zirconia, magnesia; the weight ratio of the yttrium oxide to the zirconium dioxide to the magnesium oxide is (8-12) to (7-12) to 1.
7. The alumina bulletproof ceramic of claim 6, wherein the weight ratio of the yttrium oxide to the zirconium dioxide to the magnesium oxide is (9-11): (8-10): 1.
8. A method of making the alumina ballistic resistant ceramic according to any one of claims 1-7 comprising the steps of:
(1) adding 99-99.5 parts of alumina and 0.5-1 part of auxiliary agent into a ball mill for ball milling and mixing for 18-30 h;
(2) spraying the ball-milled mixture into a granulation tower, wherein the centrifugal frequency conversion of the granulation tower is 26-32HZ, the air inlet temperature is 250-280 ℃, the air outlet temperature is 100-120 ℃, and the feeding pressure is 40-60MPa, so as to obtain granulation powder;
(3) putting the granulated powder into a double-sided press die to be pressed to obtain a green body, wherein the machine tool pressure tonnage of the double-sided press is 150-1500 tons;
(4) and (3) putting the green bodies into a normal-pressure electric push plate kiln, keeping 0.5-5cm of gap arrangement among the green bodies, controlling the temperature and the heating time of ten stages of the electric push plate kiln, sintering and cooling to obtain the aluminum oxide bulletproof ceramic.
9. The preparation method of the alumina bulletproof ceramic, according to the claim 8, is characterized in that the temperature and the heating time of the electric pushing plate kiln in the step (4) are ten stages, the temperature in the first stage is increased from room temperature to 300 ℃, and the heating time is 5 h; in the second stage, the temperature is raised from 300 ℃ to 500-600 ℃, and the temperature rise time is 6 h; in the third stage, the temperature is raised from 500-1100 ℃ to 1000-1100 ℃ for 8 h; the fourth stage is heated from 1000-1100 ℃ to 1300-1400 ℃, and the heating time is 6 h; in the fifth stage, the temperature is increased from 1300 ℃ to 1400 ℃ to 1450 ℃ to 1500 ℃ for 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1500 ℃ to 1550 ℃ to 1650 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is preserved for 4h at 1550-; the eighth stage is that the temperature is reduced from 1550-1650 ℃ to 1300-1400 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300-1400 ℃ to 800-900 ℃; and in the tenth stage, stopping blowing by the blower, and naturally cooling to room temperature from 800-900 ℃.
10. The preparation method of the alumina bulletproof ceramic, according to the claim 8, is characterized in that the temperature and the heating time of the electric pushing plate kiln in the step (4) are ten stages, the temperature in the first stage is increased from room temperature to 300 ℃, and the heating time is 5 h; in the second stage, the temperature is increased from 300 ℃ to 600 ℃, and the temperature-increasing time is 6 hours; in the third stage, the temperature is raised from 600 ℃ to 1000 ℃ for 8 h; in the fourth stage, the temperature is increased from 1000 ℃ to 1300 ℃, and the temperature-increasing time is 6 hours; in the fifth stage, the temperature is increased from 1300 ℃ to 1450 ℃, and the temperature-increasing time is 5 h; in the sixth stage, the temperature is increased from 1450 ℃ to 1630 ℃, and the temperature-increasing time is 6 h; in the seventh stage, the temperature is kept at 1630 ℃ for 4 h; in the eighth stage, the temperature is reduced from 1630 ℃ to 1300 ℃, and the temperature reduction time is 2 h; stopping heating natural gas in the ninth stage, and cooling from 1300 ℃ to 900 ℃; and in the tenth stage, stopping the blower, and naturally cooling the blower from 900 ℃ to room temperature.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007029237A2 (en) * 2005-09-08 2007-03-15 Imi Tami Institute For Research And Development Ltd. Improved alumina based ceramic objects
CN104446383A (en) * 2013-09-22 2015-03-25 扬州三山工业陶瓷有限公司 Large-size alumina integral ceramic arched plate and manufacturing method thereof
CN108164254A (en) * 2018-02-01 2018-06-15 湖南中泰特种装备有限责任公司 A kind of bulletproof ceramic sheet with cyclic structure, shellproof target plate and preparation method thereof
CN108794045A (en) * 2018-07-10 2018-11-13 武汉科技大学 A kind of high toughness aluminium oxide base bulletproof ceramic and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007029237A2 (en) * 2005-09-08 2007-03-15 Imi Tami Institute For Research And Development Ltd. Improved alumina based ceramic objects
CN104446383A (en) * 2013-09-22 2015-03-25 扬州三山工业陶瓷有限公司 Large-size alumina integral ceramic arched plate and manufacturing method thereof
CN108164254A (en) * 2018-02-01 2018-06-15 湖南中泰特种装备有限责任公司 A kind of bulletproof ceramic sheet with cyclic structure, shellproof target plate and preparation method thereof
CN108794045A (en) * 2018-07-10 2018-11-13 武汉科技大学 A kind of high toughness aluminium oxide base bulletproof ceramic and preparation method thereof

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Application publication date: 20220920