CN103382099A - Sandwich structure bulletproof ceramic sheet and low temperature sintering preparation method - Google Patents

Sandwich structure bulletproof ceramic sheet and low temperature sintering preparation method Download PDF

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CN103382099A
CN103382099A CN2013102933297A CN201310293329A CN103382099A CN 103382099 A CN103382099 A CN 103382099A CN 2013102933297 A CN2013102933297 A CN 2013102933297A CN 201310293329 A CN201310293329 A CN 201310293329A CN 103382099 A CN103382099 A CN 103382099A
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周泽华
易于
王泽华
王国伟
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Hohai University HHU
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Abstract

本发明涉及一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为85-95%Al2O3+5-15%ZrO2,中心层成分按质量百分比为75-85%Al2O3+15-25%ZrO2;烧结后三明治结构防弹陶瓷片的表面层与中心层的厚度比为1:5-15;防弹陶瓷片的表面为正六边形或正方形,厚度方向为三明治层状结构,烧结后正六边形对角线长40-60mm,厚度7-12mm,或正方形边长为30-60mm,厚度7-12mm;烧结后防弹陶瓷片的相对密度98.5-99.5%,抗冲击韧性1-1.4J,抗弯强度500-600MPa,断裂韧性8-11MPa·m1/2。可作为人体、装甲的硬质防弹材料使用。通过对氧化铝-氧化锆复合陶瓷引入三明治结构,保证相邻层间一定成分差异,使陶瓷片具有优秀抗冲击性能;并引入三步成型法,在大气环境、较低温度下完成陶瓷片的致密化。

Figure 201310293329

The invention relates to a bulletproof ceramic sheet with a sandwich structure . The composition is 75-85% Al 2 O 3 +15-25% ZrO 2 by mass percentage; the thickness ratio of the surface layer to the central layer of the bullet-proof ceramic sheet with a sandwich structure after sintering is 1:5-15; the surface of the bullet-proof ceramic sheet is Regular hexagon or square, with a sandwich layered structure in the thickness direction, after sintering, the diagonal length of the regular hexagon is 40-60mm, and the thickness is 7-12mm, or the side length of the square is 30-60mm, and the thickness is 7-12mm; bulletproof ceramics after sintering The relative density of the sheet is 98.5-99.5%, the impact toughness is 1-1.4J, the bending strength is 500-600MPa, and the fracture toughness is 8-11MPa·m 1/2 . It can be used as hard bulletproof material for human body and armor. By introducing a sandwich structure to the alumina-zirconia composite ceramics, a certain difference in composition between adjacent layers is ensured, so that the ceramic sheet has excellent impact resistance; and a three-step molding method is introduced to complete the ceramic sheet in an atmospheric environment and at a lower temperature. densification.

Figure 201310293329

Description

一种三明治结构的防弹陶瓷片及低温烧结制备方法Bulletproof ceramic sheet with sandwich structure and preparation method thereof by low-temperature sintering

  the

技术领域    technical field

本发明涉及一种特殊结构的防弹陶瓷材料及其制备方法,具体是一种具有三明治结构的氧化物防弹陶瓷片及低温烧结的制备方法。本发明主要用于防护产品中的硬质防弹材料,属于防护材料技术领域。 The invention relates to a bullet-proof ceramic material with a special structure and a preparation method thereof, in particular to an oxide bullet-proof ceramic sheet with a sandwich structure and a preparation method for low-temperature sintering. The invention is mainly used for hard bulletproof materials in protective products, and belongs to the technical field of protective materials.

背景技术 Background technique

随着军事科学技术的进步,子弹类攻击性武器的性能大幅提高,对人体和装备的威胁越来越大。从人体和装备的防护角度出发,要求防弹材料具有更高的防护效果和更加经济合理的制造手段。针对弹速快、爆破力高的子弹冲击,仅仅依靠软质防护材料对能量的缓冲和分散是不可靠的,硬质防护材料在许多防护场合的使用,如装甲防护等是必不可少的。其中,陶瓷类材料是硬质防弹材料的典型代表。 With the advancement of military science and technology, the performance of bullet-type offensive weapons has been greatly improved, and the threat to the human body and equipment is increasing. From the perspective of human body and equipment protection, bulletproof materials are required to have higher protection effects and more economical and reasonable manufacturing methods. For the impact of bullets with fast bullet speed and high explosive force, it is unreliable to rely solely on soft protective materials to buffer and disperse energy. Hard protective materials are indispensable in many protective occasions, such as armor protection. Among them, ceramic materials are typical representatives of hard bulletproof materials.

氧化铝基复合陶瓷由于具有低密度、高强度和硬度,制备工艺简单,在硬质防弹材料领域得到了广泛的应用。然而,由于其较低的韧性和相应较低的抗冲击性能,只能作为低等级防护的硬质防弹材料,或作为面板材料,配合其它背板材料复合构成结构复杂、成本较高的防弹材料。而目前用于较高等级防护的陶瓷类材料以纤维增强碳化硼或碳化硅为主。如专利“整体弧形大尺寸氧化铝防弹陶瓷板及其模具和制法”(201110088420.6)就是通过氧化铝面板与其它材料的背板复合构成;专利“碳化硼基复合防弹陶瓷及其制备方法”(200610042047.X)借助添加碳化硅晶须制备碳化硼复合防弹陶瓷,晶须分散工艺相对复杂,对设备和产品稳定性要求高,并需要借助气氛和压力完成烧结,制备成本较高。 Alumina-based composite ceramics have been widely used in the field of hard bulletproof materials due to their low density, high strength and hardness, and simple preparation process. However, due to its low toughness and correspondingly low impact resistance, it can only be used as a hard bulletproof material for low-level protection, or as a panel material, combined with other backplane materials to form a complex structure and high cost bulletproof material . At present, the ceramic materials used for higher-level protection are mainly fiber-reinforced boron carbide or silicon carbide. For example, the patent "Integral arc-shaped large-size alumina bulletproof ceramic plate and its mold and manufacturing method" (201110088420.6) is composed of an alumina panel and a back plate of other materials; the patent "boron carbide-based composite bulletproof ceramics and its preparation method" (200610042047.X) By adding silicon carbide whiskers to prepare boron carbide composite bulletproof ceramics, the whisker dispersion process is relatively complicated, which requires high equipment and product stability, and requires atmosphere and pressure to complete sintering, and the preparation cost is high.

此外,按照氧化铝基防弹陶瓷的常规烧结方法,即其在大气环境下烧结,通常的烧结温度较高,即使添加合适的助烧剂,通常的烧结致密温度也在1600℃以上,否则陶瓷很难致密。而采用放电等离子烧结(SPS)或热等静压烧结(HIP)等技术,虽然烧结温度可大幅下降,但相应的成本非常高,且工艺复杂。专利“纳米碳化硅增韧氧化铝防弹陶瓷的制备方法”(200910015239.5)中涉及的烧结温度为1650-1700℃,据分析,且使用的是气氛保护工艺。 In addition, according to the conventional sintering method of alumina-based bulletproof ceramics, that is, they are sintered in the atmosphere, the usual sintering temperature is relatively high, even if a suitable sintering aid is added, the usual sintering densification temperature is above 1600°C, otherwise the ceramics will be very Difficult to densify. However, using technologies such as spark plasma sintering (SPS) or hot isostatic pressing (HIP), although the sintering temperature can be greatly reduced, the corresponding cost is very high and the process is complicated. The sintering temperature involved in the patent "Preparation Method of Nano-Silicon Carbide Toughened Alumina Bulletproof Ceramics" (200910015239.5) is 1650-1700°C. According to the analysis, the atmosphere protection process is used.

发明内容 Contents of the invention

本发明的目的是提供一种三明治结构的防弹陶瓷片及其低温烧结制备方法,通过对氧化铝-氧化锆复合陶瓷进行成分设计和结构设计,陶瓷片表面为硬质防弹陶瓷片常用的正六边形或正方形,在与冲击面垂直方向引入三明治层状结构,并保证相邻层之间一定的成分差异,以期在烧结过程中获得合适的热失配从而提高其抗冲击性能和其它机械性能;并在制备工艺中引入三步成型法,即模压预压-模压终压-冷等静压,最终在大气环境、1520-1620℃的较低烧结温度下完成复合陶瓷的致密化过程。获得的防弹陶瓷片具有以下性能特征:相对密度98.5-99.5%,抗冲击韧性1-1.4J,抗弯强度500-600MPa,断裂韧性8-11 MPa·m1/2;可作为硬质防弹材料使用。 The purpose of the present invention is to provide a bullet-proof ceramic sheet with a sandwich structure and its low-temperature sintering preparation method. By designing the composition and structure of the alumina-zirconia composite ceramic, the surface of the ceramic sheet is a regular hexagon commonly used for hard bullet-proof ceramic sheets. Shape or square, introduce a sandwich layered structure in the direction perpendicular to the impact surface, and ensure a certain composition difference between adjacent layers, in order to obtain a suitable thermal mismatch during the sintering process to improve its impact resistance and other mechanical properties; And a three-step molding method is introduced in the preparation process, namely molding pre-pressing-molding final pressing-cold isostatic pressing, and finally the densification process of the composite ceramics is completed in the atmospheric environment and at a relatively low sintering temperature of 1520-1620°C. The obtained bulletproof ceramic sheet has the following performance characteristics: relative density 98.5-99.5%, impact toughness 1-1.4J, bending strength 500-600MPa, fracture toughness 8-11 MPa m 1/2 ; it can be used as hard bulletproof material use.

本发明实现上述目的的技术方案如下: The technical scheme that the present invention realizes above-mentioned object is as follows:

一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为85-95%Al2O3+5-15%ZrO2,中心层成分按质量百分比为75-85% Al2O3+15-25%ZrO2;烧结后三明治结构的防弹陶瓷片的表面层与中心层的厚度比为1:5-15;防弹陶瓷片的表面为正六边形或正方形,厚度方向为三明治层状结构,烧结后正六边形对角线长40-60mm,厚度7-12mm,或正方形边长为30-60mm,厚度7-12mm;烧结后防弹陶瓷片的相对密度98.5-99.5%,抗冲击韧性1-1.4J,抗弯强度500-600MPa,断裂韧性8-11 MPa·m1/2A bullet-proof ceramic sheet with a sandwich structure, characterized in that the composition of the upper and lower surface layers of the bullet-proof ceramic sheet with a sandwich structure is 85-95% Al 2 O 3 +5-15% ZrO 2 by mass percentage, and the composition of the center layer is by mass The percentage is 75-85% Al 2 O 3 +15-25% ZrO 2 ; the thickness ratio of the surface layer to the center layer of the bulletproof ceramic sheet with a sandwich structure after sintering is 1:5-15; the surface of the bulletproof ceramic sheet is regular hexagonal Shape or square, the thickness direction is a sandwich layered structure, the diagonal length of the regular hexagon after sintering is 40-60mm, the thickness is 7-12mm, or the side length of the square is 30-60mm, the thickness is 7-12mm; the bulletproof ceramic sheet after sintering The relative density is 98.5-99.5%, the impact toughness is 1-1.4J, the bending strength is 500-600MPa, and the fracture toughness is 8-11 MPa·m 1/2 .

所述的三明治结构的防弹陶瓷片,其特征在于,该防弹陶瓷片的上下表面层Al2O3含量高于中心层Al2O3含量,上下表面层ZrO2含量低于中心层ZrO2含量,以保证在烧结过程中获得合适的热失配,从而提高防弹陶瓷片抗冲击性能。 The bulletproof ceramic sheet with a sandwich structure is characterized in that the Al2O3 content of the upper and lower surface layers of the bulletproof ceramic sheet is higher than the Al2O3 content of the center layer, and the ZrO2 content of the upper and lower surface layers is lower than the ZrO2 content of the center layer. , to ensure proper thermal mismatch in the sintering process, thereby improving the impact resistance of the bulletproof ceramic sheet.

所述的三明治结构的防弹陶瓷片的制备方法,其制备步骤如下: The preparation method of the bulletproof ceramic sheet of the described sandwich structure, its preparation steps are as follows:

(1)复合粉末的配制:按质量百分比分别配制85-95% Al2O3+5-15%ZrO2和75-85% Al2O3+15-25%ZrO2复合粉末,分别经球磨混料、干燥、研磨后分别备用; (1) Preparation of composite powders: 85-95% Al 2 O 3 +5-15% ZrO 2 and 75-85% Al 2 O 3 +15-25% ZrO 2 composite powders were respectively prepared according to mass percentage, and ball milled respectively After mixing, drying and grinding, they are used separately;

(2)三明治结构防弹陶瓷片坯体的成型:本陶瓷片坯体按模压预压-模压终压-冷等静压的三步加压法成型;根据三明治结构的层状陶瓷的表面层与中心层的厚度比计算出的表面层和中心层粉末质量,按顺序依次将质量百分比为85-95% Al2O3+5-15%ZrO2复合粉末、75-85% Al2O3+15-25%ZrO2复合粉末、85-95% Al2O3+ 5-15% ZrO2复合粉末倒入预制的模具中,并在每次粉末倒入后施加20-50MPa的压力预压成型,再最终施加100-150MPa的压力成型,脱模后获得坯体;坯体最终经180-220MPa冷等静压成型备用; (2) Forming of the sandwich-structure bulletproof ceramic body: the ceramic body is formed by the three-step pressing method of molding pre-pressing-molding final pressure-cold isostatic pressing; according to the surface layer of the sandwich-structured layered ceramics and The thickness of the center layer is calculated from the surface layer and center layer powder mass, and the mass percentages are 85-95% Al 2 O 3 +5-15% ZrO 2 composite powder, 75-85% Al 2 O 3 + 15-25% ZrO 2 composite powder, 85-95% Al 2 O 3 + 5-15% ZrO 2 composite powder are poured into the prefabricated mold, and a pressure of 20-50MPa is applied after each powder pouring for pre-compression molding , and finally apply a pressure of 100-150MPa to form it, and obtain the green body after demoulding; the green body is finally formed by 180-220MPa cold isostatic pressing for later use;

(3)三明治结构防弹陶瓷片的烧结:将上述坯体在1520 -1620oC 的普通大气烧结炉内烧结并保温90-180分钟。 (3) Sintering of bulletproof ceramic sheets with sandwich structure: sinter the above green body in an ordinary atmospheric sintering furnace at 1520-1620oC and keep it warm for 90-180 minutes.

所述的制备方法,其特征在于,步骤(1)所述的Al2O3和ZrO2粉末均为亚微米或微米粒径粉末,其中在Al2O3中添加少量的MgO粉末作为助烧剂,在ZrO2中添加少量的Y2O3粉末作为稳定剂。 The preparation method is characterized in that the Al 2 O 3 and ZrO 2 powders in step (1) are both submicron or micron particle size powders, wherein a small amount of MgO powder is added to Al 2 O 3 as a firing aid Agent, add a small amount of Y 2 O 3 powder in ZrO 2 as a stabilizer.

所述的制备方法,其特征在于,步骤(2)所述的成型模具为正六边形或正方形模具,尺寸按烧结收缩比计算。 The preparation method is characterized in that the forming mold in step (2) is a regular hexagonal or square mold, and the size is calculated according to the sintering shrinkage ratio.

所述的三明治结构的防弹陶瓷片,相对密度按排水法测试,抗冲击韧性按落锤法测试,抗弯强度按三点弯曲法测试,断裂韧性按压痕法测试。 For the bulletproof ceramic sheet with a sandwich structure, the relative density is tested by the drainage method, the impact toughness is tested by the drop weight method, the bending strength is tested by the three-point bending method, and the fracture toughness is tested by the indentation method.

本发明有益的效果:通过对氧化铝-氧化锆复合陶瓷进行成分设计和结构设计,在与陶瓷片冲击面垂直方向引入三明治层状结构,并保证相邻层之间一定的成分差异,在烧结过程中获得合适的热失配,获得残余压应力,使外来冲击功在层间界面和内部压应力的协同作用下得到分散和消耗,从而提高陶瓷片的抗冲击性能和其它机械性能;并在制备工艺中引入三步成型法,即模压预压-模压终压-冷等静压,最终在大气环境、1520-1620℃的较低烧结温度下完成复合陶瓷的致密化过程。获得的防弹陶瓷片相对密度大于98.5%,抗冲击韧性大于1J,抗弯强度大于500MPa,断裂韧性大于8 MPa·m1/2;可作为硬质防弹材料使用。 Beneficial effects of the present invention: through composition design and structural design of alumina-zirconia composite ceramics, a sandwich layered structure is introduced in the direction perpendicular to the impact surface of the ceramic sheet, and a certain composition difference between adjacent layers is ensured. Appropriate thermal mismatch is obtained in the process, residual compressive stress is obtained, and the external impact energy is dispersed and consumed under the synergistic effect of the interlayer interface and internal compressive stress, thereby improving the impact resistance and other mechanical properties of the ceramic sheet; and in A three-step molding method is introduced into the preparation process, namely pre-molding-final pressing-cold isostatic pressing, and finally the densification process of the composite ceramics is completed in an atmospheric environment and at a relatively low sintering temperature of 1520-1620°C. The relative density of the obtained bulletproof ceramic sheet is greater than 98.5%, the impact toughness is greater than 1J, the bending strength is greater than 500MPa, and the fracture toughness is greater than 8 MPa·m 1/2 ; it can be used as a hard bulletproof material.

  the

附图说明 Description of drawings

图1:三明治结构的层状防弹陶瓷片设计示意图;图中表面层与中心层厚度比d1:d2=1:5-15,总厚度d=7-12mm; Figure 1: Schematic diagram of the design of a layered bulletproof ceramic sheet with a sandwich structure; in the figure, the thickness ratio of the surface layer to the central layer is d 1 : d 2 =1:5-15, and the total thickness d=7-12mm;

图2:烧结后防弹陶瓷片的界面显微形貌;界面相邻部分具有优秀的结合,无分层裂纹; Figure 2: The interface micromorphology of the bulletproof ceramic sheet after sintering; the adjacent parts of the interface have excellent bonding and no delamination cracks;

图3:防弹陶瓷片抗弯强度试验后的断口形貌;可看出清晰的解理断口,和穿晶断裂和沿晶断裂的混合断裂; Figure 3: The fracture morphology of the bulletproof ceramic sheet after the flexural strength test; it can be seen that there are clear cleavage fractures, and mixed fractures of transgranular fracture and intergranular fracture;

具体实施方式 Detailed ways

本发明通过如下措施来实现: The present invention realizes by following measures:

实施例1: Example 1:

一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为95%Al2O3+5%ZrO2,中心层成分按质量百分比为85% Al2O3+15%ZrO2;烧结后三明治结构的防弹陶瓷片的表面层与中心层的厚度比为1:12;防弹陶瓷片的表面为正六边形,厚度方向为三明治层状结构,烧结后正六边形对角线长50mm,厚度10mm;烧结后防弹陶瓷片的相对密度99.5%,抗冲击韧性1.4J,抗弯强度577MPa,断裂韧性10.56 MPa·m1/2A bullet-proof ceramic sheet with a sandwich structure, characterized in that the composition of the upper and lower surface layers of the bullet-proof ceramic sheet with a sandwich structure is 95% Al 2 O 3 +5% ZrO 2 by mass percentage, and the composition of the center layer is 85% by mass percentage Al 2 O 3 +15%ZrO 2 ; the thickness ratio of the surface layer to the center layer of the bullet-proof ceramic sheet with a sandwich structure after sintering is 1:12; the surface of the bullet-proof ceramic sheet is a regular hexagon, and the thickness direction is a sandwich layer structure. After sintering, the diagonal length of the regular hexagon is 50mm, and the thickness is 10mm; the relative density of the bulletproof ceramic sheet after sintering is 99.5%, the impact toughness is 1.4J, the bending strength is 577MPa, and the fracture toughness is 10.56 MPa·m 1/2 .

其制备步骤如下: Its preparation steps are as follows:

(1)复合粉末的配制:按质量百分比分别配制95%Al2O3+5%ZrO2和85% Al2O3+15%ZrO2复合粉末,经球磨混料、干燥、研磨后备用;其中Al2O3和ZrO2粉末粒径分别为4和0.6微米,其中Al2O3中包含质量百分比为0.5%的MgO粉末作为助烧剂,ZrO2中包含质量百分比为3%的Y2O3粉末作为稳定剂; (1) Preparation of composite powder: 95% Al 2 O 3 +5% ZrO 2 and 85% Al 2 O 3 +15% ZrO 2 composite powders were prepared respectively according to the mass percentage, mixed by ball milling, dried and ground for later use; The particle sizes of Al 2 O 3 and ZrO 2 powders are 4 and 0.6 microns respectively, wherein Al 2 O 3 contains 0.5% by mass of MgO powder as a sintering aid, and ZrO 2 contains 3% by mass of Y 2 O 3 powder as a stabilizer;

(2)三明治结构陶瓷防弹片坯体的成型:本陶瓷片坯体按模压预压-模压终压-冷等静压的三步加压法成型;根据三明治结构的层状陶瓷的表面层与中心层的厚度比计算出的表面层和中心层粉末质量,按顺序依次将一定质量的95%Al2O3+5%ZrO2复合粉末、85% Al2O3+15%ZrO2复合粉末、95%Al2O3+5%ZrO2复合粉末倒入预制的正六边形模具中,并在每次粉末倒入后施加20MPa的压力预压成型,再最终施加130MPa的压力成型,脱模后获得坯体;坯体最终经200MPa冷等静压成型备用; (2) Forming of sandwich-structure ceramic bullet-proof body: the ceramic body is formed by a three-step pressing method of molding pre-pressing-molding final pressure-cold isostatic pressing; according to the surface layer of the sandwich structure layered ceramics and The thickness of the central layer is calculated according to the surface layer and central layer powder mass, and a certain mass of 95% Al 2 O 3 +5% ZrO 2 composite powder, 85% Al 2 O 3 +15% ZrO 2 composite powder is added in sequence , 95%Al 2 O 3 +5%ZrO 2 composite powder is poured into a prefabricated regular hexagonal mold, and a pressure of 20MPa is applied after each powder is poured into the mold, and finally a pressure of 130MPa is applied for molding, demoulding Finally, the green body is obtained; the green body is finally formed by 200MPa cold isostatic pressing for standby;

(3)三明治层状结构防弹片的烧结:将坯体在1560oC 的普通大气烧结炉内烧结并保温120分钟。 (3) Sintering of bullet-proof sheet with sandwich layer structure: Sinter the green body in an ordinary atmospheric sintering furnace at 1560oC and keep it warm for 120 minutes.

上述三明治结构的防弹陶瓷片,相对密度按排水法测试,抗冲击韧性按落锤法测试,抗弯强度按三点弯曲法测试,断裂韧性按压痕法测试。 For the above-mentioned bulletproof ceramic sheet with a sandwich structure, the relative density is tested by the drainage method, the impact toughness is tested by the drop weight method, the flexural strength is tested by the three-point bending method, and the fracture toughness is tested by the indentation method.

  the

实施例2: Example 2:

一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为85%Al2O3+15%ZrO2,中心层成分按质量百分比为75% Al2O3+25%ZrO2;烧结后三明治结构的防弹陶瓷片的表面层与中心层的厚度比为1:6;防弹陶瓷片的表面为正六边形,厚度方向为三明治层状结构,烧结后正六边形对角线长40mm,厚度8mm;烧结后防弹陶瓷片的相对密度98.5%,抗冲击韧性1.0J,抗弯强度514MPa,断裂韧性9.88 MPa·m1/2A bullet-proof ceramic sheet with a sandwich structure, characterized in that the composition of the upper and lower surface layers of the bullet-proof ceramic sheet with a sandwich structure is 85% Al 2 O 3 +15% ZrO 2 by mass percentage, and the composition of the center layer is 75% by mass percentage Al 2 O 3 +25%ZrO 2 ; the thickness ratio of the surface layer to the central layer of the bullet-proof ceramic sheet with a sandwich structure after sintering is 1:6; the surface of the bullet-proof ceramic sheet is a regular hexagon, and the thickness direction is a sandwich layer structure. After sintering, the diagonal length of the regular hexagon is 40mm, and the thickness is 8mm; the relative density of the bulletproof ceramic sheet after sintering is 98.5%, the impact toughness is 1.0J, the bending strength is 514MPa, and the fracture toughness is 9.88 MPa·m 1/2 .

其制备步骤如下: Its preparation steps are as follows:

(1)复合粉末的配制:按质量百分比分别配制85%Al2O3+15%ZrO2和75% Al2O3+25%ZrO2复合粉末,经球磨混料、干燥、研磨后备用;其中Al2O3和ZrO2粉末粒径分别为4和0.6微米,其中Al2O3中包含质量百分比为0.5%的MgO粉末作为助烧剂,ZrO2中包含质量百分比为3%的Y2O3粉末作为稳定剂; (1) Preparation of composite powder: 85% Al 2 O 3 +15% ZrO 2 and 75% Al 2 O 3 +25% ZrO 2 composite powders were prepared respectively according to mass percentage, mixed by ball milling, dried and ground for later use; The particle sizes of Al 2 O 3 and ZrO 2 powders are 4 and 0.6 microns respectively, wherein Al 2 O 3 contains 0.5% by mass of MgO powder as a sintering aid, and ZrO 2 contains 3% by mass of Y 2 O 3 powder as a stabilizer;

(2)三明治层状结构防弹片坯体的成型:本陶瓷片坯体按模压预压-模压终压-冷等静压的三步加压法成型;根据三明治结构的层状陶瓷的表面层与中心层的厚度比计算出的表面层和中心层粉末质量,按顺序依次将一定质量的85%Al2O3+15%ZrO2复合粉末、75% Al2O3+25%ZrO2复合粉末、85%Al2O3+15%ZrO2复合粉末倒入预制的正六边形模具中,并在每次粉末倒入后施加50MPa的压力预压成型,再最终施加150MPa的压力成型,脱模后获得坯体;坯体最终经220MPa冷等静压成型备用; (2) Forming of the bullet-proof sheet body with a sandwich layered structure: the ceramic sheet body is formed according to the three-step pressing method of molding pre-pressing-molding final pressure-cold isostatic pressing; according to the surface layer of the sandwich-structured layered ceramic The mass of the surface layer and the center layer powder calculated by the ratio of the thickness of the center layer to the composite powder of 85% Al 2 O 3 +15% ZrO 2 and 75% Al 2 O 3 +25% ZrO 2 in sequence Powder, 85%Al 2 O 3 + 15%ZrO 2 composite powder was poured into a prefabricated regular hexagonal mold, and a pressure of 50MPa was applied for pre-compression molding after each powder pouring, and finally a pressure of 150MPa was applied for molding. After molding, the green body is obtained; the green body is finally formed by 220MPa cold isostatic pressing for later use;

(3)三明治层状结构防弹片的烧结:将坯体在1540 oC 的普通大气烧结炉内烧结并保温180分钟。 (3) Sintering of bullet-proof sheet with sandwich layered structure: the green body was sintered in an ordinary atmospheric sintering furnace at 1540 oC and kept for 180 minutes.

上述三明治结构的防弹陶瓷片,相对密度按排水法测试,抗冲击韧性按落锤法测试,抗弯强度按三点弯曲法测试,断裂韧性按压痕法测试。 For the above-mentioned bulletproof ceramic sheet with a sandwich structure, the relative density is tested by the drainage method, the impact toughness is tested by the drop weight method, the flexural strength is tested by the three-point bending method, and the fracture toughness is tested by the indentation method.

  the

实施例3: Example 3:

一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为90%Al2O3+10%ZrO2,中心层成分按质量百分比为80% Al2O3+20%ZrO2;烧结后三明治结构的防弹陶瓷片的表面层与中心层的厚度比为1:10;防弹陶瓷片的表面为正方形,厚度方向为三明治层状结构,烧结后正方形边长40mm,厚度10mm;烧结后防弹陶瓷片的相对密度99%,抗冲击韧性1.2J,抗弯强度507MPa,断裂韧性10.44MPa·m1/2A bullet-proof ceramic sheet with a sandwich structure, characterized in that the composition of the upper and lower surface layers of the bullet-proof ceramic sheet with a sandwich structure is 90% Al 2 O 3 +10% ZrO 2 by mass percentage, and the composition of the center layer is 80% by mass percentage Al 2 O 3 +20%ZrO 2 ; after sintering, the thickness ratio of the surface layer to the central layer of the bulletproof ceramic sheet with a sandwich structure is 1:10; the surface of the bulletproof ceramic sheet is square, and the thickness direction is a sandwich layered structure. The side length of the square is 40mm, and the thickness is 10mm; the relative density of the sintered bulletproof ceramic sheet is 99%, the impact toughness is 1.2J, the bending strength is 507MPa, and the fracture toughness is 10.44MPa·m 1/2 .

其制备步骤如下: Its preparation steps are as follows:

(1)复合粉末的配制:按质量百分比分别配制90%Al2O3+10%ZrO2和80% Al2O3+20%ZrO2复合粉末,经球磨混料、干燥、研磨后备用;其中Al2O3和ZrO2粉末粒径分别为4和0.6微米,其中Al2O3中包含质量百分比为0.5%的MgO粉末作为助烧剂,ZrO2中包含质量百分比为3%的Y2O3粉末作为稳定剂; (1) Preparation of composite powder: 90% Al 2 O 3 +10% ZrO 2 and 80% Al 2 O 3 +20% ZrO 2 composite powders were prepared respectively according to the mass percentage, and were mixed by ball milling, dried and ground for later use; The particle sizes of Al 2 O 3 and ZrO 2 powders are 4 and 0.6 microns respectively, wherein Al 2 O 3 contains 0.5% by mass of MgO powder as a sintering aid, and ZrO 2 contains 3% by mass of Y 2 O 3 powder as a stabilizer;

(2)三明治层状结构防弹片坯体的成型:本陶瓷片坯体按模压预压-模压终压-冷等静压的三步加压法成型;根据三明治结构的层状陶瓷的表面层与中心层的厚度比计算出的表面层和中心层粉末质量,按顺序依次将一定质量的90%Al2O3+10%ZrO2复合粉末、80% Al2O3+20%ZrO2复合粉末、90%Al2O3+10%ZrO2复合粉末倒入预制的正方形模具中,并在每次粉末倒入后施加30MPa的压力预压成型,再最终施加100MPa的压力成型,脱模后获得坯体;坯体最终经180MPa冷等静压成型备用; (2) Forming of the bullet-proof sheet body with a sandwich layered structure: the ceramic sheet body is formed according to the three-step pressing method of molding pre-pressing-molding final pressure-cold isostatic pressing; according to the surface layer of the sandwich-structured layered ceramic The surface layer and center layer powder mass calculated from the thickness ratio of the center layer, and a certain mass of 90% Al 2 O 3 + 10% ZrO 2 composite powder, 80% Al 2 O 3 + 20% ZrO 2 are compounded in sequence Powder, 90%Al 2 O 3 +10%ZrO 2 composite powder is poured into a prefabricated square mold, and a pressure of 30MPa is applied for pre-compression molding after each powder pouring, and finally a pressure of 100MPa is applied for molding. After demolding Obtain the green body; the green body is finally formed by 180MPa cold isostatic pressing for standby;

(3)三明治层状结构防弹片的烧结:将坯体在1600oC 的普通大气烧结炉内烧结并保温90分钟。 (3) Sintering of bullet-proof sheet with sandwich layered structure: Sinter the green body in an ordinary atmospheric sintering furnace at 1600oC and keep it warm for 90 minutes.

上述三明治结构的防弹陶瓷片,相对密度按排水法测试,抗冲击韧性按落锤法测试,抗弯强度按三点弯曲法测试,断裂韧性按压痕法测试。 For the above-mentioned bulletproof ceramic sheet with a sandwich structure, the relative density is tested by the drainage method, the impact toughness is tested by the drop weight method, the flexural strength is tested by the three-point bending method, and the fracture toughness is tested by the indentation method.

Claims (4)

1.一种三明治结构的防弹陶瓷片,其特征在于,三明治结构的防弹陶瓷片上下两个表面层成分按质量百分比为85-95%Al2O3+5-15%ZrO2,中心层成分按质量百分比为75-85% Al2O3+15-25%ZrO2;烧结后三明治结构防弹陶瓷片的表面层与中心层的厚度比为1:5-15;防弹陶瓷片的表面为正六边形或正方形,厚度方向为三明治层状结构,烧结后正六边形对角线长40-60mm,厚度7-12mm,或正方形边长为30-60mm,厚度7-12mm;烧结后防弹陶瓷片的相对密度98.5-99.5%,抗冲击韧性1-1.4J,抗弯强度500-600MPa,断裂韧性8-11 MPa·m1/21. A bullet-proof ceramic sheet with a sandwich structure, characterized in that the composition of the upper and lower surface layers of the bullet-proof ceramic sheet with a sandwich structure is 85-95% Al 2 O 3 +5-15% ZrO 2 by mass percentage, and the composition of the center layer The mass percentage is 75-85% Al 2 O 3 +15-25% ZrO 2 ; after sintering, the thickness ratio of the surface layer to the central layer of the bullet-proof ceramic sheet of sandwich structure is 1:5-15; the surface of the bullet-proof ceramic sheet is positive six Polygonal or square, with a sandwich layered structure in the thickness direction, after sintering, the diagonal length of a regular hexagon is 40-60mm, and the thickness is 7-12mm, or the side length of a square is 30-60mm, and the thickness is 7-12mm; after sintering, the bulletproof ceramic sheet The relative density is 98.5-99.5%, the impact toughness is 1-1.4J, the bending strength is 500-600MPa, and the fracture toughness is 8-11 MPa·m 1/2 . 2.如权利要求1所述的三明治结构的防弹陶瓷片,其特征在于,该防弹陶瓷片的上下表面层Al2O3含量高于中心层Al2O3含量,上下表面层ZrO2含量低于中心层ZrO2含量,以保证在烧结过程中获得合适的热失配,从而提高防弹陶瓷片抗冲击性能。 2. the bulletproof ceramic sheet of sandwich structure as claimed in claim 1, is characterized in that, the upper and lower surface layers Al of this bulletproof ceramic sheet O 3 content is higher than center layer Al 2 O 3 content, upper and lower surface layer ZrO content is low The content of ZrO 2 in the center layer is used to ensure proper thermal mismatch during sintering, thereby improving the impact resistance of the bulletproof ceramic sheet. 3.一种制备三明治结构的防弹陶瓷片的方法,其制备步骤如下: 3. A method for preparing a bulletproof ceramic sheet of a sandwich structure, the preparation steps of which are as follows: (1)复合粉末的配制:按质量百分比分别配制85-95% Al2O3+5-15%ZrO2和75-85% Al2O3+15-25%ZrO2复合粉末,分别经球磨混料、干燥、研磨后分别备用; (1) Preparation of composite powders: 85-95% Al 2 O 3 +5-15% ZrO 2 and 75-85% Al 2 O 3 +15-25% ZrO 2 composite powders were respectively prepared according to mass percentage, and ball milled respectively After mixing, drying and grinding, they are used separately; (2)三明治结构防弹陶瓷片坯体的成型:本陶瓷片坯体按模压预压-模压终压-冷等静压的三步加压法成型;根据三明治结构的层状陶瓷的表面层与中心层的厚度比计算出的表面层和中心层粉末质量,按顺序依次将质量百分比为85-95% Al2O3+5-15%ZrO2复合粉末、75-85% Al2O3+15-25%ZrO2复合粉末、85-95% Al2O3+ 5-15% ZrO2复合粉末倒入预制的模具中,并在每次粉末倒入后施加20-50MPa的压力预压成型,再最终施加100-150MPa的压力成型,脱模后获得坯体;坯体最终经180-220MPa冷等静压成型备用; (2) Forming of the sandwich-structure bulletproof ceramic body: the ceramic body is formed by the three-step pressing method of molding pre-pressing-molding final pressure-cold isostatic pressing; according to the surface layer of the sandwich-structured layered ceramics and The thickness of the center layer is calculated from the surface layer and center layer powder mass, and the mass percentages are 85-95% Al 2 O 3 +5-15% ZrO 2 composite powder, 75-85% Al 2 O 3 + 15-25% ZrO 2 composite powder, 85-95% Al 2 O 3 + 5-15% ZrO 2 composite powder are poured into the prefabricated mold, and a pressure of 20-50MPa is applied after each powder pouring for pre-compression molding , and finally apply a pressure of 100-150MPa to form it, and obtain the green body after demoulding; the green body is finally formed by 180-220MPa cold isostatic pressing for later use; (3)三明治结构防弹陶瓷片的烧结:将上述坯体在1520-1620oC 的普通大气烧结炉内烧结并保温90-180分钟。 (3) Sintering of bulletproof ceramic sheets with sandwich structure: sinter the above green body in an ordinary atmospheric sintering furnace at 1520-1620oC and keep it warm for 90-180 minutes. 4.如权利要求3所述的制备方法,其特征在于,步骤(1)所述的Al2O3和ZrO2粉末均为亚微米或微米粒径粉末,其中在Al2O3中添加少量的MgO粉末作为助烧剂,在ZrO2中添加少量的Y2O3粉末作为稳定剂。 4. The preparation method according to claim 3, characterized in that the Al 2 O 3 and ZrO 2 powders in step (1) are both submicron or micron particle size powders, wherein a small amount of The MgO powder is used as a sintering aid, and a small amount of Y 2 O 3 powder is added to the ZrO 2 as a stabilizer.
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CN104329988A (en) * 2014-10-16 2015-02-04 湖南中泰特种装备有限责任公司 Bulletproof ceramic chip and preparation method thereof
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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
CN108164254B (en) * 2018-02-01 2024-06-25 湖南中泰特种装备有限责任公司 Bulletproof ceramic sheet with annular structure, bulletproof target plate and preparation method thereof
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CN110092645A (en) * 2019-05-24 2019-08-06 广东工业大学 A kind of composite ceramic substrate and preparation method thereof
CN110092645B (en) * 2019-05-24 2021-07-13 广东工业大学 A kind of composite ceramic substrate and preparation method thereof
CN110563461A (en) * 2019-10-11 2019-12-13 东莞市陶陶新材料科技有限公司 preparation method of ceramic composite with high impact resistance
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Application publication date: 20131106