CN113061047B - Ceramic/ceramic bulletproof material and preparation method thereof - Google Patents
Ceramic/ceramic bulletproof material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of a ceramic/ceramic bulletproof material, which comprises the following steps: (1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric; (2) Sewing 20-60 layers of the plain woven fabric obtained in the step (1) to obtain a prefabricated part; (3) Mixing the prefabricated part obtained in the step (2) with ceramic resin, and impregnating to obtain a precursor; (4) Sintering the precursor obtained in the step (3) to obtain a complex; (5) Repeating the steps (3) and (4) for at least five times on the composite obtained in the step (4) in sequence to obtain a densified composite; (6) And (4) carrying out heat treatment on the densified complex obtained in the step (5) to obtain the ceramic/ceramic bulletproof material. The invention adopts the plain weave fabric and the sewing technology, greatly enhances the integral performance of the prefabricated part, not only improves the compactness of the fabric and reduces the fiber clearance, but also is beneficial to sintering and heat treatment densification and improves the bulletproof performance.
Description
Technical Field
The invention belongs to the technical field of bulletproof materials, and particularly relates to a ceramic/pottery bulletproof material and a preparation method thereof.
Background
Bulletproof materials are mainly divided into three types, namely soft bulletproof materials, semi-hard bulletproof materials and hard bulletproof materials. The hard bulletproof material has small deformation or even no deformation compared with soft bulletproof material and semi-hard bulletproof material under the impact of bullets, so that the protection effect is better than the protection effect of the soft bulletproof material and the semi-hard bulletproof material, and the hard bulletproof material is widely applied.
The present hard bulletproof material is generally obtained by compounding a ceramic material and a fiber material, for example, patent CN108892525A describes a preparation method of a ceramic/ceramic hard bulletproof material, which comprises the following steps: s1: placing SiC ceramic fibers in three-dimensional weaving equipment, wherein the three-dimensional weaving equipment adopts an integrated forming process to prepare a bulletproof material prefabricated part; s2: the bulletproof material prefabricated part and the ceramic resin are sequentially placed into a steel high-pressure-resistant impregnation tank, after an inlet of the steel high-pressure-resistant impregnation tank is closed, the pressure in the steel high-pressure-resistant impregnation tank is adjusted to be 0.1-2 MPa, and the impregnation time is set to be 5-15 min; s3: taking out the mixture dipped in the previous step, putting the mixture consisting of the bulletproof material prefabricated part and the ceramic resin into a high-temperature sintering furnace, adjusting the pressure of the high-temperature sintering furnace to 20-30 MPa, adjusting the temperature of the high-temperature sintering furnace to 1000-1500 ℃, sintering the mixture consisting of the bulletproof material prefabricated part and the ceramic resin in the high-temperature sintering furnace for 16-20 h, and preserving heat for 1-1.5 h; s4: the processes of the step S2 and the step S3 are repeated for 5 to 10 times in sequence; s5: taking out the mixture of the preformed bulletproof material and the ceramic resin, and carrying out heat treatment on the mixture, wherein the temperature of the heat treatment is controlled to be 1500-2000 ℃, and the time of the heat treatment processing is controlled to be 1-1.5 h; s6: and after the mixture of the bulletproof material prefabricated part and the ceramic resin is naturally cooled, taking out the mixture and carrying out post-treatment on the mixture. Tests show that the density of the bulletproof material prepared by the method is more than or equal to 22kg/m 2 Although it can prevent 7.62 x 39mm rifle bullets of AK47 assault rifles and 7.62 x 51mm nato bullets of M14 automatic rifles from shooting, when the size of the bulletproof material is 250mm x 300mm, it can only prevent 3 bullets from shooting, that is, when the bullet is impacted simultaneously by multiple bullets, the integrity of the bulletproof material can not be guaranteed, which indicates that the bulletproof performance is poor. Therefore, there is a need for an improved method for the preparation of hard ballistic materials to further improve the ballistic performance of the ballistic materials.
Disclosure of Invention
The invention aims to provide a ceramic/ceramic bulletproof material and a preparation method thereof. The pottery/ceramic bulletproof material prepared by the preparation method provided by the invention has the advantages of high hardness, high bulletproof grade, good multiple bulletproof performance and the like.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a ceramic/ceramic bulletproof material, which comprises the following steps:
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Sewing 20-60 layers of the plain woven fabric obtained in the step (1) to obtain a prefabricated part;
(3) Mixing the prefabricated part obtained in the step (2) with ceramic resin, and impregnating to obtain a precursor;
(4) Sintering the precursor obtained in the step (3) to obtain a complex;
(5) Repeating the composite obtained in the step (4) for at least five times in sequence in the steps (3) and (4) to obtain a densified composite;
(6) And (4) carrying out heat treatment on the densified complex obtained in the step (5) to obtain the ceramic/ceramic bulletproof material.
Preferably, the content of the fibers in the silicon carbide ceramic fibers in the step (1) is 40-65 wt%.
Preferably, the thickness of the plain weave fabric in the step (1) is 0.2 to 0.5mm.
Preferably, the number of layers of the plain weave fabric in the step (2) is 25 to 50.
Preferably, the ceramic resin in the step (3) includes polycarbosilane and polysiloxane.
Preferably, the pressure of the impregnation in the step (3) is 0.1 to 2MPa, and the time of the impregnation is 5 to 15min.
Preferably, the sintering pressure in the step (4) is 20-30 MPa, the sintering temperature is 1000-1500 ℃, and the sintering time is 17-21.5 h.
Preferably, the number of repetitions in said step (5) is not higher than 10.
Preferably, the temperature of the heat treatment in the step (6) is 1500-2000 ℃, and the time of the heat treatment is 1-1.5 h.
The invention also provides the ceramic/ceramic bulletproof material prepared by the preparation method of the technical scheme.
The invention provides a preparation method of a ceramic/ceramic bulletproof material, which comprises the following steps: (1) Weaving the silicon carbide ceramic fiber to obtain plain weave fabric; (2) Sewing 20-60 layers of the plain woven fabric obtained in the step (1) to obtain a prefabricated part; (3) Mixing the prefabricated member obtained in the step (2) with ceramic resin, and impregnating to obtain a precursor; (4) Sintering the precursor obtained in the step (3) to obtain a complex; (5) Repeating the steps (3) and (4) for at least five times on the composite obtained in the step (4) in sequence to obtain a densified composite; (6) And (4) carrying out heat treatment on the densified complex obtained in the step (5) to obtain the ceramic/ceramic bulletproof material. The invention adopts the plain weave fabric and the sewing technology, greatly enhances the integral performance of the prefabricated part, not only can improve the compactness of the fabric so as to reduce the fiber gaps in the fabric, but also is beneficial to densifying the bulletproof material to higher density through later-stage sintering and heat treatment so as to improve the bulletproof performance of the bulletproof materialAnd (4) elastic energy. Experimental results show that the density of the pottery/ceramic bulletproof material prepared by the preparation method provided by the invention is 20-30 kg/m 2 (ii) a HV value is 1300-2000; at a density of 20kg/m 2 When the automatic rifle is used, the AK47 assault rifle 7.62X 39mm rifle bullets and M14 automatic rifle 7.62X 51mm NATO bullets can be effectively prevented, the automatic rifle meets the national NIJ010106 human body armor protection III-level standard, and the automatic rifle can prevent at least 6 bullets from shooting when the size is 250mm X300 mm.
Detailed Description
The invention provides a preparation method of a ceramic/ceramic bulletproof material, which comprises the following steps:
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Sewing 20-60 layers of the plain woven fabric obtained in the step (1) to obtain a prefabricated part;
(3) Mixing the prefabricated member obtained in the step (2) with ceramic resin, and impregnating to obtain a precursor;
(4) Sintering the precursor obtained in the step (3) to obtain a complex;
(5) Repeating the steps (3) and (4) for at least five times on the composite obtained in the step (4) in sequence to obtain a densified composite;
(6) And (4) carrying out heat treatment on the densified complex obtained in the step (5) to obtain the ceramic/ceramic bulletproof material.
The invention weaves the silicon carbide ceramic fiber to obtain plain weave fabric.
In the present invention, the fiber content in the silicon carbide ceramic fiber is preferably 40 to 65wt%, more preferably 45 to 60wt%, and still more preferably 50 to 55wt%. The source of the silicon carbide ceramic fiber is not particularly limited in the present invention, and a commercially available product known to those skilled in the art may be used.
In the present invention, the thickness of the plain weave fabric is preferably 0.2 to 0.5mm, more preferably 0.3 to 0.4mm. The weaving process of the present invention is not particularly limited, and the operation of weaving a plain woven fabric, which is well known to those skilled in the art, may be employed. In the invention, the plain weave fabric has higher compactness, can reduce fiber gaps in the fabric, and is beneficial to densifying the bulletproof material to higher density through later-stage sintering and heat treatment, thereby improving the hardness of the bulletproof material.
After obtaining the plain weave fabric, the invention carries out sewing treatment on 20-60 layers of the plain weave fabric to obtain the prefabricated member. The invention combines a plurality of layers of plain weave fabrics together by adopting a sewing technology, and can improve the Z-direction overall performance of the bulletproof material, including the performances of delamination resistance, impact resistance, bulletproof resistance and the like.
In the present invention, the number of layers of the plain weave fabric is preferably 25 to 50, more preferably 30 to 45. In the present invention, when the number of layers of the plain woven fabric is within the above range, the bulletproof effect of the bulletproof material can be further improved.
In the invention, the suture thread used for the suture treatment is preferably made of silicon carbide ceramic fiber; the preparation method of the suture line is preferably as follows:
1) Plying 2-4 silicon carbide ceramic fibers according to an S-twist twisting mode to obtain S primary twisted yarns;
2) Plying 2-4 silicon carbide ceramic fibers according to a Z-twisting mode to obtain Z primary twisted yarns;
3) Twisting and plying the S primarily-twisted yarn obtained in the step 1) and the Z primarily-twisted yarn obtained in the step 2) to obtain a suture line blank;
4) Sizing the suture blank obtained in the step 3) by using a polyvinyl alcohol glue solution, and drying to obtain a suture;
the step 1) and the step 2) are not in sequence.
The twisting mode of the S twist and the twisting mode of the Z twist are not particularly limited in the present invention, and may be any twisting mode known to those skilled in the art.
The sources of the silicon carbide ceramic fiber and the polyvinyl alcohol glue solution are not particularly limited in the invention, and commercially available products well known to those skilled in the art can be adopted. The sizing amount of the polyvinyl alcohol glue solution is not particularly limited in the invention, and the sizing amount known to those skilled in the art can be adopted. The drying operation is not particularly limited in the present invention, and a drying operation known to those skilled in the art may be employed.
In the present invention, the sewing treatment is preferably lock sewing; the ratio of the volume of the stitching thread in the preform is preferably 2 to 10%, more preferably 5 to 8%. The invention adopts lock type sewing and limits the volume ratio of the sewing line, and can further improve the Z-direction overall performance of the bulletproof material, including the performances of delamination resistance, impact resistance, bulletproof property and the like.
After the prefabricated member is obtained, the prefabricated member is mixed with ceramic resin and impregnated to obtain the precursor.
In the present invention, the ceramic resin preferably includes polycarbosilane and polysiloxane; the polycarbosilane is preferably used in an amount of 80 to 90wt%, more preferably 85wt%, and the polysiloxane is preferably used in an amount of 10 to 20wt%, more preferably 15wt%, based on 100% by mass of the ceramic resin. The source of the ceramic resin is not particularly limited in the present invention, and commercially available products known to those skilled in the art may be used. In the invention, when the ceramic resin is prepared from the above substances and the using amount, the toughness of the ceramic is improved while the hardness of the ceramic is satisfied by mixing a plurality of ceramic resins, so that the multi-bullet prevention performance of the bulletproof material is further improved.
The amount of the ceramic resin used in the present invention is not particularly limited, as long as the preform can be completely immersed in the ceramic resin during the impregnation. The operation of mixing the preform with the ceramic resin is not particularly limited in the present invention, and the operation of impregnating the preform with the resin, which is well known to those skilled in the art, may be employed.
In the present invention, the pressure of the impregnation is preferably 0.1 to 2MPa, more preferably 0.5 to 1.5MPa, and still more preferably 1 to 1.2MPa; the time for the impregnation is preferably 5 to 15min, more preferably 8 to 10min. In the present invention, when the pressure and time of the impregnation are within the above ranges, the compactness of the precursor can be further improved, thereby further improving the bonding strength of the preform with the ceramic resin.
In the present invention, the impregnation is preferably carried out in a steel high-pressure resistant impregnation tank. The type of the steel high-pressure resistant impregnation tank is not particularly limited in the present invention, and a steel high-pressure resistant impregnation tank well known to those skilled in the art may be used.
After obtaining the precursor, the invention sinters the precursor to obtain the complex. According to the invention, the precursor is sintered, so that the hardness and density of the bulletproof material can be improved, and the bulletproof effect of the bulletproof material is improved.
In the present invention, the pressure of the sintering is preferably 20 to 30MPa, more preferably 25 to 28MPa; the sintering temperature is preferably 1000-1500 ℃, and more preferably 1200-1400 ℃; the sintering time is preferably 17 to 21.5 hours, more preferably 18 to 20 hours. In the invention, when the sintering pressure, temperature and time are in the above ranges, the hardness and density of the bulletproof material can be further improved, so that the bulletproof effect of the bulletproof material is further improved.
In the present invention, the sintering is preferably performed in a high-temperature sintering furnace. The type of the high-temperature sintering furnace is not particularly limited in the present invention, and a high-temperature sintering furnace known to those skilled in the art may be used.
After obtaining the composite body, the invention repeats the impregnation step and the sintering step for at least five times in sequence to obtain the densified composite body. In the present invention, the number of repetitions is preferably not more than 10, and more preferably 5 to 9. The complex is subjected to multiple times of impregnation and sintering, so that the hardness and compactness of the bulletproof material can be further improved, and the bulletproof performance of the bulletproof material is improved.
After the densified complex is obtained, the invention carries out heat treatment on the densified complex to obtain the ceramic/ceramic bulletproof material. The heat treatment is carried out on the densified complex, so that the hardness and the densification performance of the bulletproof material can be improved, and the bulletproof material has excellent bulletproof performance, thereby meeting the bulletproof requirement.
In the present invention, the temperature of the heat treatment is preferably 1500 to 2000 ℃, more preferably 1600 to 1900 ℃, and more preferably 1700 to 1800 ℃; the time of the heat treatment is preferably 1 to 1.5 hours, more preferably 1.2 to 1.4 hours. In the present invention, the hardness and the densification property of the bulletproof material may be further improved when the temperature and time of the heat treatment are within the above ranges.
In the present invention, the heat treatment is preferably performed in an inert atmosphere; the inert atmosphere is preferably CH 4 And C 2 H 2 At least one of (1). In the present invention, the heat treatment is performed in an inert atmosphere to prevent the densified composite from being oxidized during the heat treatment and affecting the bulletproof performance.
In the present invention, the heat treatment is preferably performed in a high-temperature sintering furnace. The type of the high-temperature sintering furnace is not particularly limited in the present invention, and a high-temperature sintering furnace known to those skilled in the art may be used.
The invention adopts the plain weave fabric and the sewing technology, so that the integral performance of the prefabricated part is greatly enhanced, the compactness of the fabric can be improved, the fiber gap in the fabric is reduced, and the later sintering and heat treatment are facilitated to densify the bulletproof material to a higher density, so that the bulletproof performance of the bulletproof material is improved.
According to the invention, 20-60 layers of lamellar plain woven fabrics are integrally sewn through a sewing technology, so that the integrity of the prepared bulletproof material is better (the performances of delamination resistance, impact resistance, bulletproof resistance and the like are better), and the thickness of the prefabricated part (the thickness is 4-30 mm) can be further reduced.
The bulletproof material prepared by the preparation method provided by the invention has light weight (20-30 kg/m) 2 ) High hardness (HV value 1300-2000), high bulletproof grade (can meet the requirements of 4, 5 and 6 bulletproof of GA141-2010 standard; meets the requirements of 4-level, 5-level and 6-level bulletproof of GJB4300A-2012 standard; and the grade III bulletproof requirement of the NIJ010106 standard) and good multi-bulletproof performance, and the like, and can be used for protecting high-speed steel core bullets emitted by semi-automatic rifles, sniper rifles and the like.
The invention also provides the ceramic/ceramic bulletproof material prepared by the preparation method of the technical scheme. The ceramic/ceramic bulletproof material provided by the invention has the advantages of light weight, high hardness, high bulletproof grade, good multi-shot prevention performance and the like, and can be used for protecting high-speed steel core bullets emitted by semi-automatic rifles, sniper rifles and the like.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Performing lock stitching on 45 layers of plain weave fabrics obtained in the step (1) by adopting a silicon carbide ceramic fiber suture line to obtain a prefabricated part; wherein the volume proportion of the suture line in the prefabricated member is 2%;
(3) Dipping the prefabricated part obtained in the step (2) in ceramic resin in a steel high-pressure resistant dipping tank for 8min, wherein the dipping pressure is 1MPa, and thus obtaining a precursor; the ceramic resin comprises 80wt% of polycarbosilane and 20wt% of polysiloxane;
(4) Sintering the precursor obtained in the step (3) in a high-temperature sintering furnace at a high temperature of 1400 ℃ for 20 hours under the high pressure of 20MPa to obtain a complex;
(5) Repeating the steps (3) and (4) five times on the composite obtained in the step (4) in sequence to obtain a densified composite;
(6) Placing the densified composite obtained in the step (5) in a high-temperature sintering furnace in CH 4 And C2H 2 And carrying out heat treatment under protection to obtain the ceramic/ceramic bulletproof material, wherein the heat treatment temperature is 1700 ℃, and the time is 1h.
Example 2
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Performing lock-type sewing on 50 layers of plain woven fabrics obtained in the step (1) by adopting silicon carbide ceramic fiber sewing threads to obtain prefabricated parts; wherein the volume proportion of the suture line in the prefabricated member is 5 percent;
(3) Dipping the prefabricated part obtained in the step (2) in ceramic resin in a steel high-pressure resistant dipping tank for 10min, wherein the dipping pressure is 1.2MPa, and obtaining a precursor; the ceramic resin comprises polycarbosilane and polysiloxane, wherein the polycarbosilane accounts for 80wt%, and the polysiloxane accounts for 20wt%;
(4) Sintering the precursor obtained in the step (3) in a high-temperature sintering furnace at 1500 ℃ for 20 hours under 20MPa high pressure to obtain a complex;
(5) Repeating the steps (3) and (4) five times on the composite obtained in the step (4) in sequence to obtain a densified composite;
(6) Placing the densified complex obtained in the step (5) in a high-temperature sintering furnace in CH 4 And C 2 H 2 And under protection, carrying out heat treatment to obtain the ceramic/ceramic bulletproof material, wherein the temperature of the heat treatment is 1700 ℃, and the time is 1h.
Example 3
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Performing lock stitching on 60 layers of plain weave fabrics obtained in the step (1) by adopting a silicon carbide ceramic fiber suture line to obtain a prefabricated part; wherein the volume proportion of the suture line in the prefabricated member is 10 percent;
(3) Dipping the prefabricated part obtained in the step (2) in ceramic resin in a steel high-pressure resistant dipping tank for 15min, wherein the dipping pressure is 2MPa, and thus obtaining a precursor; the ceramic resin comprises 80wt% of polycarbosilane and 20wt% of polysiloxane;
(4) Sintering the precursor obtained in the step (3) in a high-temperature sintering furnace for 20 hours at 1500 ℃ under 25MPa high pressure to obtain a complex;
(5) Repeating the steps (3) and (4) five times on the composite obtained in the step (4) in sequence to obtain a densified composite;
(6) Placing the densified complex obtained in the step (5) in a high-temperature sintering furnace in CH 4 And C 2 H 2 Under protection, carrying out heat treatment to obtain the ceramic/ceramic bulletproof materialWherein the temperature of the heat treatment is 2000 ℃ and the time is 1.5h.
The performance tests of the ceramic/ceramic ballistic resistant materials prepared in examples 1-3 were performed and the results are shown in table 1.
TABLE 1 data for the properties of the ceramic/ceramic ballistic materials of examples 1-3
| Example 1 | Example 2 | Example 3 | |
| Density/kg/m 2 | 22 | 23 | 26 |
| HV value | 1500 | 1650 | 1875 |
The bulletproof performance of the ceramic/pottery bulletproof material prepared in examples 1 to 3 was tested and found to be 20kg/m in density 2 When the size of the bullet is 250mm multiplied by 300mm, the bullet can effectively prevent 7.62 multiplied by 39mm rifle bullets of AK47 assault rifles and 7.62 multiplied by 51mmNATO bullets of M14 automatic rifles, meets the national NIJ010106 human body armor protection III-level standard, and can prevent at least 6 bullets from shooting.
As can be seen from the above examples, the pottery/ceramic bulletproof material prepared by the preparation method provided by the invention has the advantages of high hardness, high bulletproof grade, good multi-shot bulletproof performance and the like.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. A preparation method of a ceramic/ceramic bulletproof material comprises the following steps:
(1) Weaving the silicon carbide ceramic fiber to obtain a plain weave fabric;
(2) Sewing 20-60 layers of the plain woven fabric obtained in the step (1) to obtain a prefabricated part;
(3) Mixing the prefabricated part obtained in the step (2) with ceramic resin, and impregnating to obtain a precursor;
(4) Sintering the precursor obtained in the step (3) to obtain a complex;
(5) Repeating the steps (3) and (4) for at least five times on the composite obtained in the step (4) in sequence to obtain a densified composite;
(6) Carrying out heat treatment on the densified complex obtained in the step (5) to obtain a ceramic/ceramic bulletproof material;
the ceramic resin in the step (3) is polycarbosilane and polysiloxane.
2. The method according to claim 1, wherein the silicon carbide ceramic fiber in the step (1) has a fiber content of 40 to 65wt%.
3. The production method according to claim 1, wherein the thickness of the plain woven fabric in the step (1) is 0.2 to 0.5mm.
4. The method according to claim 1, wherein the number of layers of the plain woven fabric in the step (2) is 25 to 50.
5. The method according to claim 1, wherein the pressure of the impregnation in the step (3) is 0.1 to 2MPa, and the time of the impregnation is 5 to 15min.
6. The preparation method according to claim 1, wherein the sintering pressure in the step (4) is 20-30 MPa, the sintering temperature is 1000-1500 ℃, and the sintering time is 17-21.5 h.
7. The method according to claim 1, wherein the number of repetitions in step (5) is not more than 10.
8. The method according to claim 1, wherein the temperature of the heat treatment in the step (6) is 1500 to 2000 ℃ and the time of the heat treatment is 1 to 1.5 hours.
9. A ceramic/ceramic ballistic material prepared by the process of any one of claims 1 to 8.
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