CN109049267B - A kind of multi-channel ceramic preform under the coating of Ti-Fe micropowder and its preparation method and application - Google Patents

A kind of multi-channel ceramic preform under the coating of Ti-Fe micropowder and its preparation method and application Download PDF

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CN109049267B
CN109049267B CN201811006086.3A CN201811006086A CN109049267B CN 109049267 B CN109049267 B CN 109049267B CN 201811006086 A CN201811006086 A CN 201811006086A CN 109049267 B CN109049267 B CN 109049267B
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涂小慧
李卫
郑宝超
刘侃
林怀俊
张鹏
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Jinan University
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B1/00Producing shaped prefabricated articles from the material
    • B28B1/004Devices for shaping artificial aggregates from ceramic mixtures or from mixtures containing hydraulic binder
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
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Abstract

The invention belongs to the field of material processing, and discloses a multi-channel ceramic preform coated with Ti-Fe micro powder, and a preparation method and application thereof. According to the invention, the alloy powder is obtained near the deep eutectic point of the Fe-Ti alloy by a Mechanical Alloying (MA) method, the melting temperature of the alloy powder can reach 1085 ℃, the alloy powder and ZTA ceramic particles are subjected to heat preservation at 1250-1550 ℃ by a pressureless sintering method, molten liquid Ti is promoted to perform activation treatment on the ZTA surface, the ZTA and surface activation effects can be obviously improved, a Ti-O transition layer is formed between the ceramic and the binder, so that the crushing strength of the preform is improved, the wettability of the ceramic surface and a steel solution is improved, and the crushing strength of the preform can reach 5 MPa.

Description

一种Ti-Fe微粉包覆下的多通道陶瓷预制体及其制备方法和 应用A multi-channel ceramic preform covered with Ti-Fe micropowder and its preparation method and application

技术领域technical field

本发明属于材料加工领域,特别涉及一种Ti-Fe微粉包覆下的多通道陶瓷预制体及其制备方法和应用。The invention belongs to the field of material processing, and in particular relates to a multi-channel ceramic preform under the coating of Ti-Fe micropowder and a preparation method and application thereof.

背景技术Background technique

颗粒增强钢铁基复合材料中陶瓷颗粒起到提高钢铁材料耐磨损性的作用。在服役过程中,钢铁基体支撑陶瓷颗粒,使其随着钢铁基体磨损量的增加突出于钢铁基体,阻挡了钢铁材料的进一步被磨损。而在制备复合材料过程中陶瓷颗粒的粘结成型,以及陶瓷颗粒与金属间的界面结合强度是复合材料性能改善的关键。The ceramic particles in particle-reinforced steel matrix composites play a role in improving the wear resistance of steel materials. During the service process, the steel matrix supports the ceramic particles, making them protrude from the steel matrix with the increase of the wear amount of the steel matrix, preventing the further wear of the steel material. In the process of preparing composite materials, the bonding and forming of ceramic particles and the interface bonding strength between ceramic particles and metals are the keys to improving the performance of composite materials.

在材料加工领域内,由于氧化锆增韧氧化铝陶瓷(ZTA)具有出色的硬韧性,被广泛的作为填充料引入到高铬铸铁、钢、高锰钢以及部分硬质合金中。并且其较好的经济适用性,也有利于材料的规模化和批量化生产;特别在材料的减磨,抗磨方面,ZTA颗粒常作为金属材料的抗磨增强相,用来提高材料的抗冲击磨损性能。另外,在钢铁冶炼过程中,时常采用微纳米尺度的ZTA陶瓷微粉作为孕育剂,起到细化晶粒的作用,提高了材料整体机械性能的目的。然而,由于ZTA陶瓷界面稳定性好,成型困难,与钢铁熔体之间的润湿性极低等特点,成为钢铁基陶瓷复合材料发展的主要瓶颈。In the field of material processing, zirconia toughened alumina ceramics (ZTA) have been widely introduced as fillers into high-chromium cast iron, steel, high-manganese steel and some cemented carbides due to their excellent hardness and toughness. And its better economical applicability is also conducive to the large-scale and mass production of materials; especially in terms of material wear reduction and anti-wear, ZTA particles are often used as anti-wear enhancement phases of metal materials to improve the material's resistance to wear. Impact wear performance. In addition, in the process of iron and steel smelting, micro-nano-scale ZTA ceramic powder is often used as an inoculant to refine the grains and improve the overall mechanical properties of the material. However, due to the good interfacial stability of ZTA ceramics, the difficulty of forming, and the extremely low wettability with steel melt, it has become the main bottleneck for the development of steel-based ceramic composites.

陶瓷颗粒与金属间界面的结合方式决定着所形成的界面的结合强度,目前陶瓷颗粒与金属间界面主要以机械结合为主,冶金结合较难,这主要是由于陶瓷和金属截然不同的化学性能、热膨胀系数等特性,因而导致陶瓷颗粒与金属间界面的不良结合。另外,ZTA陶瓷预制体主要采用机械合金化(MA)与无压烧结结合的工艺进行制备。MA工艺是利用粉体颗粒与磨球之间长时间激烈地冲击、碰撞,促使粉体间实现充分的原子扩散,无压烧结主要是将活化粉体与陶瓷表面产生原子扩散,另外使得陶瓷颗粒之间可以通过粉体的烧结而实现一定强度的连接成型。能够与陶瓷表面发生扩散反应的粉体,促使陶瓷表面具有一定的金属性,可以显著的提高陶瓷表面在金属液中的浸润性,为后续的铸渗过程中陶瓷表面与金属溶体实现充分接触。因此,亟需研发一种可与金属间界面冶金结合的陶瓷。The bonding method of the interface between ceramic particles and metal determines the bonding strength of the interface formed. At present, the interface between ceramic particles and metal is mainly mechanical bonding, and metallurgical bonding is difficult. This is mainly due to the completely different chemical properties of ceramics and metals. , thermal expansion coefficient and other characteristics, resulting in poor bonding between the ceramic particles and the metal interface. In addition, ZTA ceramic preforms are mainly prepared by a combination of mechanical alloying (MA) and pressureless sintering. The MA process uses the long-term intense impact and collision between the powder particles and the grinding ball to promote sufficient atomic diffusion between the powders. Pressureless sintering mainly generates atomic diffusion between the activated powder and the ceramic surface, and also makes the ceramic particles A certain strength can be achieved through the sintering of the powder. The powder that can have a diffusion reaction with the ceramic surface promotes the ceramic surface to have a certain metallicity, which can significantly improve the wettability of the ceramic surface in the molten metal, and achieve full contact between the ceramic surface and the metal solution in the subsequent casting infiltration process. Therefore, there is an urgent need to develop a ceramic that can be metallurgically bonded to the metal-to-metal interface.

发明内容SUMMARY OF THE INVENTION

为了克服上述现有技术的缺点与不足,本发明的首要目的在于提供一种Ti-Fe微粉包覆下的多通道陶瓷预制体的制备方法。该方法通过合金化处理Fe-Ti混合粉体,Ti含量控制在25-35wt%区间,将粉体与陶瓷进行混合烧结,可实现陶瓷颗粒间较高的结合强度,预制体的压溃强度可达5MPa,添加的Ti粉与ZTA陶瓷中的O结合,对陶瓷表面形成有效的活化作用。In order to overcome the above-mentioned shortcomings and deficiencies of the prior art, the primary purpose of the present invention is to provide a method for preparing a multi-channel ceramic preform covered by Ti-Fe micropowder. In this method, the Fe-Ti mixed powder is alloyed, the Ti content is controlled in the range of 25-35wt%, and the powder and the ceramic are mixed and sintered to achieve high bonding strength between the ceramic particles, and the crushing strength of the preform can be improved. Up to 5MPa, the added Ti powder combines with O in the ZTA ceramics to form an effective activation effect on the ceramic surface.

本发明另一目的在于提供上述方法制备的Ti-Fe微粉包覆下的多通道陶瓷预制体。Another object of the present invention is to provide a multi-channel ceramic preform under the coating of Ti-Fe micropowder prepared by the above method.

本发明再一目的在于提供上述Ti-Fe微粉包覆下的多通道陶瓷预制体在制备高铬铸铁基或高锰钢基等钢铁基复合材料中的应用。Another object of the present invention is to provide the application of the multi-channel ceramic preform covered by the above-mentioned Ti-Fe micropowder in the preparation of high-chromium cast iron-based or high-manganese steel-based steel-based composite materials.

本发明的目的通过下述方案实现:The object of the present invention is realized through the following scheme:

一种Ti-Fe微粉包覆下的多通道陶瓷预制体的制备方法,其主要包括以下步骤:A preparation method of a multi-channel ceramic preform under the coating of Ti-Fe micropowder, which mainly comprises the following steps:

(1)混粉并合金化:将还原铁粉和Ti粉混合,然后加入到球磨罐中球磨进行合金化,得混合粉体粘结剂;(1) Mixing powder and alloying: mixing reduced iron powder and Ti powder, then adding it into a ball mill tank for alloying by ball milling to obtain a mixed powder binder;

(2)混料:将步骤(1)中得到的混合粉体粘结剂与ZTA颗粒混合,然后加入水玻璃作为固化剂和石蜡颗粒作为造孔剂,搅拌使粉末粘结剂均匀包覆在ZTA陶瓷颗粒表面,得混合物料;(2) Mixing: mixing the mixed powder binder obtained in step (1) with ZTA particles, then adding water glass as a curing agent and paraffin particles as a pore-forming agent, stirring to make the powder binder evenly coated on the Surface of ZTA ceramic particles to obtain mixed material;

(3)固化:将步骤(2)中得到的混合物料填充到成型模具中,通过紧固磨具将预制体定形和紧实,持续通入CO2气体进行固化,然后烘干脱模即得固化成型后的预制体;(3) curing: filling the mixture obtained in step (2) into the forming mold, fixing and compacting the preform by tightening the abrasive tool, continuously introducing CO gas for curing, and then drying and demoulding. Preform after curing and molding;

(4)真空无压烧结:将步骤(3)中固化成型后的预制体放入真空烧结炉中进行烧结即得具有一定强度和孔隙率的陶瓷预制体。(4) Vacuum pressureless sintering: put the solidified preform in step (3) into a vacuum sintering furnace for sintering to obtain a ceramic preform with certain strength and porosity.

为防止球磨后的混合粉末比表面积增加,易与空气中的氧发生反应,通常步骤(1)和步骤(2)均在保护气体下进行,所述的保护气体可为氩气或氮气中的一种;In order to prevent the specific surface area of the mixed powder after ball milling from increasing, and it is easy to react with oxygen in the air, usually step (1) and step (2) are carried out under protective gas, and the protective gas can be argon or nitrogen. A sort of;

步骤(1)中所述的还原铁粉的纯度为99.99%,粒度小于等于100目;Ti粉的纯度99.99%,粒度小于等于300目;The purity of the reduced iron powder described in the step (1) is 99.99%, and the particle size is less than or equal to 100 mesh; the purity of the Ti powder is 99.99%, and the particle size is less than or equal to 300 mesh;

步骤(1)中所述的还原铁粉和Ti粉的用量控制在Ti-Fe共晶区域成分附近,优选为Ti粉占还原铁粉和Ti粉的总质量的25~35wt%;The amount of the reduced iron powder and Ti powder described in the step (1) is controlled near the composition of the Ti-Fe eutectic region, preferably, the Ti powder accounts for 25-35wt% of the total mass of the reduced iron powder and the Ti powder;

步骤(1)中所述的球磨机优选行星式球磨机,球磨工艺为:球磨时间为24~30h,磨球直径为5~10mm,磨球与混合粉末的重量比为10:1,球磨机转速为300~450r/min。The ball mill described in the step (1) is preferably a planetary ball mill, and the ball milling process is as follows: the ball milling time is 24-30 h, the diameter of the grinding ball is 5-10 mm, the weight ratio of the grinding ball to the mixed powder is 10:1, and the ball mill rotating speed is 300 ~450r/min.

步骤(2)中所述的ZTA陶瓷颗粒的粒径为8~10目;步骤(2)中所述的石蜡颗粒的粒径为10~12目;The particle size of the ZTA ceramic particles described in the step (2) is 8 to 10 meshes; the particle size of the paraffin wax particles described in the step (2) is 10 to 12 meshes;

步骤(2)中所述的混合粉体的用量为步骤(2)中所得混合物料总重量的3~8wt%;步骤(2)所述的水玻璃(Na2SiO3·9H2O)的用量为步骤(2)中所述的合金粉体重量的3~7%,优选为5%;步骤(2)中所述的石蜡颗粒的用量为步骤(2)中所得混合物料总重量的1~3wt%;所述的ZTA颗粒为余量;The dosage of the mixed powder described in the step (2) is 3 to 8 wt % of the total weight of the mixed material obtained in the step (2); the amount of the water glass (Na 2 SiO 3 ·9H 2 O) described in the step (2) is The dosage is 3-7% of the weight of the alloy powder described in the step (2), preferably 5%; the dosage of the paraffin particles described in the step (2) is 1% of the total weight of the mixture obtained in the step (2). ~3wt%; the ZTA particles are the remainder;

步骤(2)中所述的搅拌是为了使原料之间混合均匀,本领域常规使用的转速都可以实现本步骤的目的,因此可不用限定搅拌速度,优选用玻璃棒搅拌5~15min;The stirring described in the step (2) is to make the raw materials evenly mixed, and the rotating speed conventionally used in the art can achieve the purpose of this step, so there is no need to limit the stirring speed, preferably a glass rod is used to stir for 5 to 15 min;

步骤(3)中所述的成型模具优选为30mm×20mm×10mm空心立方体,中间存在Φ10mm圆柱体构成,模具为木质纤维材料,通过紧固螺栓连接各个分段模块。The molding die described in step (3) is preferably a 30mm×20mm×10mm hollow cube with a Φ10mm cylinder in the middle, the die is made of wood fiber material, and each segmented module is connected by fastening bolts.

步骤(3)中所述的紧固是指将放入模具中的混料通过模具的中线对中合缝,然后紧固螺栓即可。The tightening described in step (3) refers to aligning the mixture put into the mold through the center line of the mold, and then tightening the bolts.

步骤(3)中所述的持续通入CO2是指将装有混合物的成型模具置于一个出气孔打开的容器中,充气速率为40~60cm3/s,充气时间为0.5~1h,进气管的管直径55~59mm,出气孔的管直径要大于进气孔管直径,但要小于100mm。The continuous introduction of CO 2 in the step (3) refers to placing the molding die with the mixture in a container with an open air outlet, the inflation rate is 40-60 cm 3 /s, the inflation time is 0.5-1 h, and the The diameter of the trachea is 55-59mm, and the diameter of the air outlet is larger than that of the air inlet, but less than 100mm.

步骤(3)中所述的烘干是指在60~80℃的真空干燥箱中保温1~2h;The drying described in step (3) refers to keeping the temperature in a vacuum drying oven at 60-80° C. for 1-2 hours;

步骤(4)中所述的烧结是指烧结过程真空度保持在2.9×10-3Pa,烧结保温温度控制在1250~1550℃,保温1h,随炉冷却到室温。The sintering described in step (4) means that the vacuum degree during the sintering process is kept at 2.9×10 -3 Pa, and the sintering holding temperature is controlled at 1250-1550° C. for 1 hour, and then cooled to room temperature with the furnace.

一种由上述方法制备得到的Ti-Fe微粉包覆下的多通道陶瓷预制体。A multi-channel ceramic preform under the coating of Ti-Fe micropowder prepared by the above method.

上述的Ti-Fe微粉包覆下的多通道陶瓷预制体在制备高铬铸铁基或高锰钢基等钢铁基复合材料中的应用。The application of the multi-channel ceramic preform under the coating of the above-mentioned Ti-Fe micropowder in the preparation of high-chromium cast iron-based or high-manganese steel-based steel-based composite materials.

本发明的机理为:The mechanism of the present invention is:

Ti与O具有良好的结合特性,然而纯的Ti熔点1670℃,远高于钢铁材料的熔化温度,不利于与ZTA中的氧结合,对ZTA表面活化作用下降,本发明通过机械合金化(MA)的方法获得Fe-Ti合金深共晶点附近得合金粉体,合金粉体的熔化温度可达1085℃,通过无压烧结的方法将合金粉体与ZTA陶瓷颗粒在1250~1550℃保温,促使熔融液态Ti对ZTA表面进行活化处理,可以显著提高ZTA表面活化作用,陶瓷与粘结剂间形成了Ti-O过渡层使得预制体的压溃强度增加,提高陶瓷表面与钢铁溶液的润湿性,预制体的压溃强度可达5MPa。Ti and O have good bonding characteristics, but pure Ti has a melting point of 1670 ° C, which is much higher than the melting temperature of steel materials, which is not conducive to bonding with oxygen in ZTA, and has a reduced surface activation effect on ZTA. ) method to obtain the alloy powder near the deep eutectic point of Fe-Ti alloy, the melting temperature of the alloy powder can reach 1085 ℃, and the alloy powder and ZTA ceramic particles are kept at 1250-1550 ℃ by the pressureless sintering method, Promote the activation of the ZTA surface by molten Ti, which can significantly improve the ZTA surface activation. A Ti-O transition layer is formed between the ceramic and the binder, which increases the crushing strength of the preform and improves the wetting of the ceramic surface and the iron and steel solution. The crushing strength of the preform can reach 5MPa.

本发明相对于现有技术,具有如下的优点及有益效果:Compared with the prior art, the present invention has the following advantages and beneficial effects:

(1)Fe-Ti微粉作为陶瓷颗粒的粘结剂可以与陶瓷表面的原子形成扩散反应,能够极大的改善陶瓷表面的反应特性,预制体的强度和成型能力得到改善。(1) Fe-Ti micropowder, as a binder of ceramic particles, can form a diffusion reaction with the atoms on the ceramic surface, which can greatly improve the reaction characteristics of the ceramic surface, and the strength and formability of the preform are improved.

(2)预制体在定型固化过程中,固化剂与CO2的反应可以对预制体进行定型处理,可加快具有复杂结构的预制体的定型,该方法适用于对预制体成型能力要求较高的金属基复合材料的制备,可以显著提高预制体的定型效率和复杂型体的成型能力。(2) During the shaping and curing process of the preform, the reaction between the curing agent and CO2 can shape the preform, which can speed up the shaping of the preform with complex structure. The preparation of metal matrix composites can significantly improve the shaping efficiency of preforms and the forming ability of complex shapes.

(3)通过石蜡颗粒的添加可以提高预制体的空隙形成能力,增加预制体的蜂窝状多孔特性,提高ZTA陶瓷的浸润能力。(3) The addition of paraffin particles can improve the void formation ability of the preform, increase the honeycomb porous characteristics of the preform, and improve the infiltration ability of ZTA ceramics.

附图说明Description of drawings

图1为实施例1中制备的Ti-Fe微粉包覆下的多通道陶瓷预制体的照片图;Fig. 1 is a photograph of the multi-channel ceramic preform under the coating of Ti-Fe micropowder prepared in Example 1;

图2为实施例1中烧结后预制体中陶瓷颗粒与粘结剂的背散射图像以及过渡层的EDS线扫描图。2 is a backscattered image of the ceramic particles and the binder in the preform after sintering in Example 1 and an EDS line scan image of the transition layer.

图3为实施例1中烧结后ZTA陶瓷表面与高铬铸铁间润湿角测试图。3 is a test chart of the wetting angle between the ZTA ceramic surface and high-chromium cast iron after sintering in Example 1.

具体实施方式Detailed ways

下面结合实施例和附图对本发明作进一步详细的描述,但本发明的实施方式不限于此。The present invention will be described in further detail below with reference to the embodiments and accompanying drawings, but the embodiments of the present invention are not limited thereto.

实施例中所用试剂如无特殊说明均可从市场常规购得。实施例中所用的球磨机为YXQM行星式球磨机。The reagents used in the examples can be routinely purchased from the market unless otherwise specified. The ball mill used in the examples is a YXQM planetary ball mill.

预制体的孔隙率通过以阿基米德排水法测试得到,具体计算步骤如下:陶瓷预制体的空隙为开气孔,通过阿基米德法测量气孔所占材料整体的体积百分比,以P表示孔隙率。试验中采用水煮法测定预制体的孔隙率。首先称量需要的试样干重,记为m0;将称量完地试样放入干净的烧杯中,往杯中注入蒸馏水,直至淹没试样。接着将烧杯置于电炉上加热至沸腾,并保持沸腾状态1-2h,使蒸馏水完全渗透至预制体的空隙内。然后停止加热使其降至室温。接着把试样快速取出放入事先准备好称重用的天平托盘中,称取饱和试样在水中的悬浮重m1;将饱和试样取出,拭去饱和试样表面的水,快速称量饱和试样的质量m2,通过公式算出孔隙率P。The porosity of the preform is measured by the Archimedes drainage method. The specific calculation steps are as follows: The voids of the ceramic preform are open pores, and the volume percentage of the pores occupied by the whole material is measured by the Archimedes method, and the pores are represented by P. Rate. In the test, the porosity of the preform was determined by the boiling method. First, weigh the required dry weight of the sample, denoted as m 0 ; put the weighed sample into a clean beaker, and pour distilled water into the beaker until the sample is submerged. Next, place the beaker on an electric furnace and heat it to boiling, and keep it in a boiling state for 1-2 hours, so that the distilled water can completely penetrate into the voids of the preform. Then stop heating and let it come down to room temperature. Then quickly take out the sample and put it into the balance tray prepared in advance for weighing, and weigh the suspension weight m 1 of the saturated sample in water; take out the saturated sample, wipe off the water on the surface of the saturated sample, and quickly weigh the saturated sample. For the mass m 2 of the sample, the porosity P is calculated by the formula.

P=(m2-m0)/(m2-m1)P=(m 2 -m 0 )/(m 2 -m 1 )

预制体的压溃强度通过以下步骤测试得到:将制备的中空的圆柱形ZTA陶瓷预制体置于试验机的两平板之间,使试样的轴线与平板平行。无振动地连续加载,加载速度0.5MPa/s-3MPa/s之间,加载时间10s,压溃强度根据公式:The crush strength of the preform was measured by the following steps: The prepared hollow cylindrical ZTA ceramic preform was placed between two flat plates of the testing machine, so that the axis of the sample was parallel to the flat plate. Continuous loading without vibration, loading speed between 0.5MPa/s-3MPa/s, loading time 10s, crush strength according to the formula:

K=F(D-e)/Le2 K=F(De)/Le 2

式中:K—径向压溃强度,单位为兆帕(MPa);Where: K—radial crushing strength, in megapascals (MPa);

F--压溃负荷,单位为牛(N);F - crushing load, the unit is Newton (N);

L—试样长度,单位为毫米(mm);L—the length of the sample, in millimeters (mm);

D—试样外径,单位为毫米(mm);D—the outer diameter of the sample, in millimeters (mm);

e—试样壁厚,单位为毫米(mm)。e—the wall thickness of the sample, in millimeters (mm).

实施例1:Example 1:

(1)取纯度99.99%,粒度100~200目,还原Fe粉与纯度为99.99%,粒度300目的Ti粉,按Ti粉占Ti粉和铁粉总重量的30wt.%进行混粉,然后加入到球磨罐中进行球磨合金化,球磨工艺为:球料比10:1,转速300r/min,球磨时间24h,使Fe,Ti粉体实现均匀混合,得到粉体粘结剂。(1) Take the purity of 99.99%, the particle size of 100-200 mesh, the reduced Fe powder and the Ti powder with a purity of 99.99% and a particle size of 300 mesh, and mix the powder according to the total weight of the Ti powder and the iron powder. Go to the ball milling tank for ball milling and alloying. The ball milling process is as follows: the ratio of ball to material is 10:1, the rotation speed is 300r/min, and the ball milling time is 24h, so that Fe and Ti powders can be uniformly mixed to obtain powder binder.

球磨后的混合粉末粒度变小,表面能急剧增大,粉体极易与空气中的氧发生反应,因此需在通入有惰性气体的手套箱中取出粉末;The particle size of the mixed powder after ball milling becomes smaller, the surface energy increases sharply, and the powder easily reacts with oxygen in the air, so it is necessary to take out the powder in a glove box with inert gas;

(2)在30mm×20mm×10mm空心立方体,中间存在Φ10mm圆柱体构成的模具中,选取粒径8~10目的ZTA陶瓷颗粒(ZrO2占20wt.%,Al2O3占80wt.%)30g,Ti-Fe混合微粉2.4g,水玻璃的量为0.12g,10~12目的石蜡颗粒作为造孔剂加入0.65g。用玻璃棒搅拌10min,使粘结剂均匀地包覆在ZTA颗粒表面,整个过程均在N2保护气氛中进行。(2) In a mold composed of a 30mm×20mm×10mm hollow cube with a Φ10mm cylinder in the middle, select 30g of ZTA ceramic particles with a particle size of 8-10 mesh (ZrO 2 accounts for 20wt.%, Al 2 O 3 accounts for 80wt.%) , 2.4g of Ti-Fe mixed micropowder, 0.12g of water glass, and 0.65g of 10-12 mesh paraffin wax particles as a pore-forming agent. Stir with a glass rod for 10 min to make the binder evenly coat the surface of the ZTA particles, and the whole process is carried out in a N2 protective atmosphere.

(3)将预制体放入手套箱中,打开出气孔,并充入CO2气体,气体通入时间0.5h,充气速率为50cm3/s,待预制体固化成型后,将模具置入60℃的恒温炉中,保温30min进行烘干,将预制体脱模取出。(3) Put the preform into the glove box, open the air outlet, and fill with CO 2 gas, the gas introduction time is 0.5h, and the inflation rate is 50 cm 3 /s. After the preform is cured and formed, the mold is placed in 60 In a constant temperature furnace at ℃, the temperature is kept for 30 minutes for drying, and the preform is demolded and taken out.

(4)预制体采用无压烧结制备烧结过程的真空度保持在2.9×10-3Pa,烧结保温温度为1300℃,保温时间1h,随炉冷却到室温制备出表面活化的多通道的ZTA陶瓷预制体。(4) The preform was prepared by pressureless sintering. The vacuum degree of the sintering process was kept at 2.9×10 -3 Pa, the sintering holding temperature was 1300 ℃, the holding time was 1 h, and the surface-activated multi-channel ZTA ceramics were prepared by cooling to room temperature with the furnace. prefab.

图1为实施例中所得ZTA陶瓷预制体的照片图。FIG. 1 is a photograph of the ZTA ceramic preform obtained in the example.

图2为实施例1中烧结后预制体中陶瓷颗粒与粘结剂的背散射图像以及过渡层的EDS线扫描图,从图2中可以看出,ZTA陶瓷中的氧和粉体粘结剂中的Ti是形成过渡层的主要成分,Ti与ZTA陶瓷中的O反应生成氧化物,对陶瓷表面出现失氧区,这些区域形成有效的活化;陶瓷与粘结剂间形成2um~8um的Ti-O过渡层,陶瓷颗粒间结合强度较高,未发现明显开裂现象,预制体的孔隙率60%,压溃强度5MPa。Figure 2 is the backscattered image of the ceramic particles and the binder in the preform after sintering in Example 1 and the EDS line scan of the transition layer. It can be seen from Figure 2 that the oxygen and powder binder in the ZTA ceramic Ti is the main component to form the transition layer. Ti reacts with O in ZTA ceramics to form oxides, and there are oxygen loss areas on the surface of the ceramics, and these areas form effective activation; 2um ~ 8um of Ti is formed between the ceramics and the binder. -O transition layer, the bonding strength between ceramic particles is high, no obvious cracking phenomenon is found, the porosity of the preform is 60%, and the crushing strength is 5MPa.

图3为实施例1中烧结后ZTA表面与金属高铬铸铁润湿角的测量结果,可以看出润湿角小于15.1°,陶瓷表面显现出较好的润湿效果,表明烧结后的ZTA陶瓷表面可以被耐磨钢液体较好的润湿,可以在复合界面形成有效的结合或者元素的扩散,有利于冶金界面的形成。Figure 3 shows the measurement results of the wetting angle between the ZTA surface and metallic high-chromium cast iron after sintering in Example 1. It can be seen that the wetting angle is less than 15.1°, and the ceramic surface shows a good wetting effect, indicating that the sintered ZTA ceramic The surface can be well wetted by wear-resistant steel liquid, which can form effective bonding or element diffusion at the composite interface, which is beneficial to the formation of metallurgical interface.

实施例2Example 2

(1)将球磨罐放入手套箱中,通入惰性气体,取纯度99.99%、粒度100-200目的还原Fe粉与纯度为99.99%、粒度300目的Ti粉,按Ti粉占Ti粉和铁粉总重量比25wt.%进行混粉;将球磨罐进行紧固密封,在YXQM行星式球磨机中合金化处理,其中磨球球径10mm,球料比10:1,转速300r/min,球磨时间24h,使Fe,Ti粉体实现充分的反应,得到粉体粘结剂。(1) Put the ball mill tank into the glove box, pass in the inert gas, and take the reduced Fe powder with a purity of 99.99% and a particle size of 100-200 meshes and a Ti powder with a purity of 99.99% and a particle size of 300 meshes. The total weight ratio of powder is 25wt.% for powder mixing; the ball mill tank is tightly sealed and alloyed in a YXQM planetary ball mill, wherein the grinding ball diameter is 10mm, the ball-to-material ratio is 10:1, the rotation speed is 300r/min, and the ball milling time 24h, the Fe and Ti powders were fully reacted to obtain powder binders.

由于球磨后的混合粉末粒度变小,表面能急剧增大,粉体极易与空气中的氧发生反应,因此将球磨罐仍然放入充满惰性气体的手套箱中进行开罐取粉,并且将取出来的合金粉末放入密闭的容器中保存;Since the particle size of the mixed powder after ball milling becomes smaller, the surface energy increases sharply, and the powder easily reacts with oxygen in the air. Therefore, the ball mill jar is still placed in a glove box filled with inert gas to open the jar to collect the powder, and the The extracted alloy powder is stored in a closed container;

(2)在30mm×20mm×10mm空心立方体,中间存在Φ10mm圆柱体构成的模具中,选取粒径8~10目的ZTA陶瓷颗粒(ZrO2占20wt.%,Al2O3占80wt.%)30g,Ti-Fe混合微粉2.4g,水玻璃的量为0.12g,10~12目的石蜡颗粒作为造孔剂加入0.65g。用玻璃棒搅拌10min,是粘结剂均匀地包覆在ZTA颗粒表面,整个过程均在N2保护气氛中进行。(2) In a mold composed of a 30mm×20mm×10mm hollow cube with a Φ10mm cylinder in the middle, select 30g of ZTA ceramic particles with a particle size of 8-10 mesh (ZrO 2 accounts for 20wt.%, Al 2 O 3 accounts for 80wt.%) , 2.4g of Ti-Fe mixed micropowder, 0.12g of water glass, and 0.65g of 10-12 mesh paraffin wax particles as a pore-forming agent. Stir with a glass rod for 10 min, the binder is evenly coated on the surface of the ZTA particles, and the whole process is carried out in a N2 protective atmosphere.

(3)将预制体放入手套箱中,打开出气孔,并充入CO2气体的,气体通入时间0.5h,充气速率为50cm3/s,待预制体固化成型后,将模具置入60℃的恒温炉中,保温30min进行烘干,将预制体脱模取出。(3) Put the preform into the glove box, open the air outlet, and fill with CO 2 gas, the gas introduction time is 0.5h, and the inflation rate is 50 cm 3 /s. After the preform is cured and formed, the mold is placed in the In a constant temperature furnace at 60°C, hold the temperature for 30 minutes for drying, and then demould the preform.

(4)预制体采用无压烧结制备,烧结过程的真空度保持在2.9×10-3Pa,烧结温度为1250℃,保温时间1h,随炉冷却到室温制备出表面活化的多通道的ZTA陶瓷预制体。(4) The preform was prepared by pressureless sintering, the vacuum degree of the sintering process was kept at 2.9×10 -3 Pa, the sintering temperature was 1250°C, the holding time was 1h, and the surface-activated multi-channel ZTA ceramics were prepared by cooling to room temperature with the furnace. prefab.

所得ZTA陶瓷预制体,从烧结后预制体中陶瓷颗粒与粘结剂的背散射图像以及过渡层的EDS线扫描图可以判断,陶瓷颗粒与粘结剂间形成约1um~3um的Ti-O过渡层,预制体的孔隙率62%,压溃强度1MPa。The obtained ZTA ceramic preform can be judged from the backscattered image of the ceramic particles and the binder in the sintered preform and the EDS line scan image of the transition layer, and a Ti-O transition of about 1um to 3um is formed between the ceramic particles and the binder. layer, the porosity of the preform is 62%, and the crushing strength is 1MPa.

实施例2中烧结后ZTA表面与金属高铬铸铁润湿角也小于15.1°,说明本实施例烧结后的ZTA陶瓷表面可以被耐磨钢液体较好的润湿,可以在复合界面形成有效的结合或者元素的扩散,有利于冶金界面的形成。In Example 2, the wetting angle between the ZTA surface and the metallic high-chromium cast iron after sintering is also less than 15.1°, which shows that the ZTA ceramic surface after sintering in this example can be well wetted by the wear-resistant steel liquid, and can form an effective composite interface. Bonding or diffusion of elements favors the formation of metallurgical interfaces.

实施例3:Example 3:

(1)取纯度99.99%,粒度100-200目,还原Fe粉与纯度为99.99%,粒度300目的Ti粉,按Ti粉占Ti粉和铁粉总重量的35wt.%进行混粉,然后加入到球磨罐中进行球磨合金化,球磨工艺为:球料比10:1,转速300r/min,球磨时间为24h,使Fe,Ti粉体实现均匀混合,得到粉体粘结剂。(1) Take the purity of 99.99%, the particle size of 100-200 mesh, the reduced Fe powder and the Ti powder with a purity of 99.99% and a particle size of 300 mesh, and mix the powder according to the total weight of the Ti powder and the iron powder by 35wt.%, and then add Go to the ball milling tank for ball milling alloying. The ball milling process is as follows: the ratio of ball to material is 10:1, the rotation speed is 300r/min, and the ball milling time is 24h, so that Fe and Ti powders can be uniformly mixed to obtain powder binder.

球磨后的混合粉末粒度变小,表面能急剧增大,粉体极易与空气中的氧发生反应,因此需在通入有惰性气体的手套箱中取出粉末;The particle size of the mixed powder after ball milling becomes smaller, the surface energy increases sharply, and the powder easily reacts with oxygen in the air, so it is necessary to take out the powder in a glove box with inert gas;

(2)在30mm×20mm×10mm空心立方体,中间存在Φ10mm圆柱体构成的模具中,选取粒径8~10目的ZTA陶瓷颗粒(ZrO2占20wt.%,Al2O3占80wt.%)30g,Ti-Fe混合微粉2.4g,水玻璃的量为0.12g,10~12目的石蜡颗粒作为造孔剂加入0.65g。用玻璃棒搅拌10min,是粘结剂均匀地包覆在ZTA颗粒表面,整个过程均在N2保护气氛中进行。(2) In a mold composed of a 30mm×20mm×10mm hollow cube with a Φ10mm cylinder in the middle, select 30g of ZTA ceramic particles with a particle size of 8-10 mesh (ZrO 2 accounts for 20wt.%, Al 2 O 3 accounts for 80wt.%) , 2.4g of Ti-Fe mixed micropowder, 0.12g of water glass, and 0.65g of 10-12 mesh paraffin wax particles as a pore-forming agent. Stir with a glass rod for 10 min, the binder is evenly coated on the surface of the ZTA particles, and the whole process is carried out in a N2 protective atmosphere.

(3)将预制体放入手套箱中,打开出气孔,并充入CO2气体的,气体通入时间0.5h,充气速率为50cm3/s,待预制体固化成型后,将模具置入60℃的恒温炉中,保温30min进行烘干,将预制体脱模取出。(3) Put the preform into the glove box, open the air outlet, and fill with CO 2 gas, the gas introduction time is 0.5h, and the inflation rate is 50 cm 3 /s. After the preform is cured and formed, the mold is placed in the In a constant temperature furnace at 60°C, hold the temperature for 30 minutes for drying, and then demould the preform.

(4)预制体采用无压烧结制备,烧结过程的真空度保持在2.9×10-3Pa,烧结保温温度为1300℃,保温时间1h,随炉冷却到室温制备出表面活化的多通道的ZTA陶瓷预制体。(4) The preform was prepared by pressureless sintering, the vacuum degree of the sintering process was kept at 2.9×10 -3 Pa, the sintering holding temperature was 1300 ℃, the holding time was 1 h, and the surface-activated multi-channel ZTA was prepared by cooling to room temperature with the furnace Ceramic preforms.

所得ZTA陶瓷预制体,通过烧结后预制体中陶瓷颗粒与粘结剂的背散射图像以及过渡层的EDS线扫描图可以确定,陶瓷与粘结剂间形成2um-5um的Ti-O过渡层,陶瓷颗粒间结合强度较高,未发现明显开裂现象,预制体的孔隙率61%,压溃强度5MPa。The obtained ZTA ceramic preform can be determined from the backscattering image of the ceramic particles and the binder in the sintered preform and the EDS line scan of the transition layer. A 2um-5um Ti-O transition layer is formed between the ceramic and the binder. The bonding strength between ceramic particles is high, and no obvious cracking phenomenon is found. The porosity of the preform is 61%, and the crushing strength is 5MPa.

实施例3中烧结后ZTA表面与金属高铬铸铁润湿角也小于15.1°,说明本实施例烧结后的ZTA陶瓷表面可以被耐磨钢液体较好的润湿,可以在复合界面形成有效的结合或者元素的扩散,有利于冶金界面的形成。In Example 3, the wetting angle between the ZTA surface and the metallic high-chromium cast iron after sintering is also less than 15.1°, which indicates that the ZTA ceramic surface after sintering in this example can be well wetted by the wear-resistant steel liquid, and can form an effective composite interface. Bonding or diffusion of elements favors the formation of metallurgical interfaces.

上述实施例为本发明较佳的实施方式,但本发明的实施方式并不受上述实施例的限制,其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化,均应为等效的置换方式,都包含在本发明的保护范围之内。The above-mentioned embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above-mentioned embodiments, and any other changes, modifications, substitutions, combinations, The simplification should be equivalent replacement manners, which are all included in the protection scope of the present invention.

Claims (8)

1. A preparation method of a multi-channel ceramic preform coated by Ti-Fe micro powder is characterized by mainly comprising the following steps:
(1) mixing powder and alloying: mixing reduced iron powder and Ti powder, and adding the mixture into a ball milling tank for ball milling to alloy, thereby obtaining a mixed powder binder;
(2) mixing materials: mixing the mixed powder binder obtained in the step (1) with ZTA particles, adding water glass as a curing agent and paraffin particles as a pore-forming agent, and stirring to uniformly coat the powder binder on the surfaces of the ZTA ceramic particles to obtain a mixed material;
(3) and (3) curing: filling the mixed material obtained in the step (2) into a forming die, shaping and compacting the prefabricated body by a fastening grinding tool, and continuously introducing CO2Curing the gas, drying and demoulding to obtain a cured and molded prefabricated body;
(4) vacuum pressureless sintering: placing the prefabricated body after being cured and molded in the step (3) into a vacuum sintering furnace for sintering to obtain a ceramic prefabricated body with certain strength and porosity;
the amount of the reduced iron powder and the Ti powder in the step (1) is 25-35 wt% of the total mass of the reduced iron powder and the Ti powder;
the ball milling process in the step (1) comprises the following steps: the ball milling time is 24-30 h, the diameter of the grinding ball is 5-10 mm, the weight ratio of the grinding ball to the mixed powder is 10:1, and the rotating speed of the ball mill is 300-450 r/min.
2. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
and (3) performing the step (1) and the step (2) under protective gas, wherein the protective gas is one of nitrogen or argon.
3. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the purity of the reduced iron powder in the step (1) is 99.99%, and the granularity is less than or equal to 100 meshes; the purity of Ti powder is 99.99%, and the granularity is less than or equal to 300 meshes.
4. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the using amount of the mixed powder in the step (2) is 3-8 wt% of the total weight of the mixed material obtained in the step (2); the amount of the water glass in the step (2) is 3-7% of the weight of the alloy powder in the step (2); the dosage of the paraffin particles in the step (2) is 1-3 wt% of the total weight of the mixed material obtained in the step (2); the balance of ZTA particles.
5. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the fastening in the step (3) is to center and joint the mixed material placed in the mold through the center line of the mold, and then fasten bolts;
continuously introducing CO in the step (3)2The gas means that a mould containing the mixed material is placed in a container with an open air outlet, and the aeration rate is 40-60 cm3The inflation time is 0.5-1 h, the pipe diameter of the air inlet pipe is 55-59 mm, and the pipe diameter of the air outlet hole is larger than that of the air inlet hole but smaller than 100 mm;
and (3) drying refers to keeping the temperature in a vacuum drying oven at 60-80 ℃ for 1-2 h.
6. The method for preparing a multi-channel ceramic preform coated with Ti-Fe micropowder according to claim 1, wherein:
the sintering in the step (4) is firingThe vacuum degree in the process of forming is kept at 2.9 × 10-3Pa, controlling the sintering heat preservation temperature at 1250-1550 ℃, preserving the heat for 1h, and cooling to room temperature along with the furnace.
7. A Ti-Fe micropowder-coated multi-channel ceramic preform prepared according to the method of any one of claims 1 to 6.
8. The use of the Ti-Fe micropowder-coated multi-channel ceramic preform of claim 7 in the preparation of steel-based composites.
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