CN1312402A - Technological process of electrophoretic coprecipitation-sintering to prepare gradient metal/biological glass ceramic coating - Google Patents
Technological process of electrophoretic coprecipitation-sintering to prepare gradient metal/biological glass ceramic coating Download PDFInfo
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- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 abstract description 18
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Abstract
电泳共沉积—烧结法制备金属/生物玻璃陶瓷梯度涂层技术,采用表面改性技术,使生物玻璃(BG)颗粒和羟基磷灰石(HA)颗粒在所选合适的分散介质中具有相同的带电特性,从而实现了BG粉料和HA粉料在作为电极的基体上的共沉积;同时通过连续改变电泳液的组成,使涂层的成份产生梯度变化,由于涂层的沉积状况与两电极间的电场强度有关,通过连续改变沉积电压,可以得到具有一定孔结构梯度的涂层。电泳共沉积所制的涂层经烧结处理可得到结合强度优良的金属/生物玻璃陶瓷梯度涂层。
Electrophoretic co-deposition-sintering method to prepare metal/bioglass-ceramic gradient coating technology, using surface modification technology to make bioglass (BG) particles and hydroxyapatite (HA) particles have the same Charging characteristics, so as to realize the co-deposition of BG powder and HA powder on the substrate as the electrode; at the same time, by continuously changing the composition of the electrophoretic liquid, the composition of the coating will change gradually. Due to the deposition status of the coating and the two electrodes By changing the deposition voltage continuously, a coating with a certain pore structure gradient can be obtained. The coating prepared by electrophoretic co-deposition can be sintered to obtain a metal/biological glass-ceramic gradient coating with excellent bonding strength.
Description
本发明涉及在各类复杂形状金属表面制备金属/生物活性玻璃/羟基磷灰石等系列梯度涂层复合材料及其制备方法。The invention relates to the preparation of a series of gradient coating composite materials such as metal/bioactive glass/hydroxyapatite and the like on metal surfaces of various complex shapes and a preparation method thereof.
在力学性能优良的基体(特别是金属基体)上制备陶瓷涂层，从而发挥基体材料和陶瓷材料的综合优势，越来越引起广泛关注。为了获得性能优良的涂层复合材料，将涂层设计成具有一定的组成和结构梯度是很有必要的。为了达到这些目标，近几年来，国内外研究出许多方法来解决涂层的问题。如：自蔓延高温合成技术(SHS)、激光溶覆法、溶胶-凝胶(Sol-Gel)法等，但这些方法存在成本高、工艺复杂等问题。目前，应用较多而又比较成熟的是等离子喷涂工艺，该方法为一线性工艺，且在喷涂过程中温度很高，其应用和涂层性能都受到较大的影响，另外，对复杂表面无法实现涂层。Preparation of ceramic coatings on substrates with excellent mechanical properties (especially metal substrates) to take advantage of the comprehensive advantages of substrate materials and ceramic materials has attracted more and more attention. In order to obtain coating composites with excellent properties, it is necessary to design the coating to have a certain composition and structure gradient. In order to achieve these goals, in recent years, many methods have been researched at home and abroad to solve the problem of coating. Such as: self-propagating high-temperature synthesis technology (SHS), laser cladding method, sol-gel (Sol-Gel) method, etc., but these methods have problems such as high cost and complicated process. At present, the plasma spraying process is widely used and relatively mature. This method is a linear process, and the temperature is very high during the spraying process. Its application and coating performance are greatly affected. In addition, it cannot be applied to complex surfaces. Achieve coating.
本发明的目的是提供一种非线性涂层工艺，可以在形状复杂和表面多孔的基体上制备出均匀涂层，该工艺具有成本低、工艺简单；可连续生产，又可间歇操作；料液可循环利用，无污染物排放；适用于大规模生产等优点——电泳共沉积-烧结法。The purpose of the present invention is to provide a kind of non-linear coating technology, can prepare uniform coating on the substrate with complex shape and surface porosity, and this technology has cost low, technology is simple; Can be produced continuously, can operate intermittently again; Recyclable, no pollutant discharge; suitable for large-scale production and other advantages - electrophoretic co-deposition - sintering method.
电泳沉积(EPD)是指电泳和沉积两个过程的综合。电泳是指在外加电场的作用下，胶体粒子在分散介质中做定向移动的现象；沉积是指微粒聚沉成较密集的质团。事实上，对于电泳液而言，并不一定要求其为胶体，通过本研究的装置，凡是由粒径小于10μm且经适当处理的粒子组成的胶体悬浮液分散体系，均适用于电泳沉积。对于胶体悬浮液分散体系，表现出来的性质与胶体分散体系是相似的，因为在胶体悬浮液分散体系中，粒子具有双电层结构，且带有动电电位，因而，在电场作用下能作定向移动，当其运动到作为电极的基体附近时，由于电解质浓度的增加，或强电场作用下双电层被压缩，其结果相当于降低了电极附近颗粒的Zeta电位，从而导致粒子发生絮凝。而此时，粒子之间距离很小，粒子之间的伦敦-范德华吸引力占主导地位，从而在基体上形成紧密堆积的涂层。通过对涂层原料颗粒表面进行协调改性处理，可使其带上同种电荷，根据其对电场的敏感程度，配合调节沉积电压，可实现不同成分的颗粒在基体上先后沉积或共同沉积，从而获得组成和孔结构呈梯度变化的涂层坯体。由电泳沉积所制得的涂层仅为较紧密堆积的坯体，涂层与基体结合强度很低，通过烧结可增强涂层与基体的结合，同时也使坯体本身致密化。梯度涂层中无明显的界面，从而使热应力得到了缓和，提高了涂层的结合强度和稳定性。这是其它涂覆工艺结合热处理所不能比拟的。Electrophoretic deposition (EPD) refers to the combination of electrophoresis and deposition. Electrophoresis refers to the phenomenon of directional movement of colloidal particles in the dispersion medium under the action of an external electric field; deposition refers to the aggregation of particles into denser mass groups. In fact, for the electrophoretic fluid, it is not necessarily required to be a colloid. Through the device of this study, any colloidal suspension dispersion system composed of properly treated particles with a particle size of less than 10 μm is suitable for electrophoretic deposition. For the colloidal suspension dispersion system, the properties exhibited are similar to those of the colloidal dispersion system, because in the colloidal suspension dispersion system, the particles have an electric double layer structure and have a zeta potential. Therefore, under the action of an electric field, they can act as Directional movement, when it moves to the vicinity of the substrate as the electrode, due to the increase of the electrolyte concentration, or the compression of the electric double layer under the action of a strong electric field, the result is equivalent to reducing the Zeta potential of the particles near the electrode, thereby causing the particles to flocculate. At this time, the distance between the particles is small, and the London-van der Waals attraction between the particles dominates, resulting in the formation of a tightly packed coating on the substrate. By coordinating and modifying the surface of coating raw material particles, it can be charged with the same kind of charge. According to its sensitivity to the electric field, with the adjustment of deposition voltage, particles of different components can be deposited successively or co-deposited on the substrate. Thus, a coated body with gradient changes in composition and pore structure is obtained. The coating prepared by electrophoretic deposition is only a relatively densely packed green body, and the bonding strength between the coating and the substrate is very low. The bonding between the coating and the substrate can be enhanced by sintering, and the green body itself is also densified. There is no obvious interface in the gradient coating, so that the thermal stress is eased, and the bonding strength and stability of the coating are improved. This is unmatched by other coating processes combined with heat treatment.
下面结合附图对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings.
图1，本发明工艺流程图；Fig. 1, process flow diagram of the present invention;
图2，本发明电泳共沉积装置示意图。Fig. 2 is a schematic diagram of the electrophoretic co-deposition device of the present invention.
(1)-直流电源(带脉冲)；(2)-电压表；(3)-电流表；(4)-阴极；(5)-阳极；(6)-加液器；(7)-电泳槽；(8)-恒流泵；(9)-调节槽；(10)-磁力搅器(带加热)。(1)-DC power supply (with pulse); (2)-Voltmeter; (3)-Ammeter; (4)-Cathode; (5)-Anode; (6)-Liquidizer; (7)-Electrophoresis tank ; (8)-constant flow pump; (9)-regulating tank; (10)-magnetic stirrer (with heating).
根据附图2，对本发明作详细的进一步说明。According to accompanying drawing 2, the present invention is further described in detail.
首先根据待制的涂层复合材料对性能的要求，对涂层组成和结构进行优化设计；然后制备涂层粉料，筛选分散介质，结合对涂层粉料在分散介质中带电特性的分析，对其进行表面改性。本发明主要以生物活性玻璃(BG)颗粒和HA颗粒作为涂层原料，在作为电极的基体(金属)上实现共沉积，然后根据涂层原料的沉积状况确定工艺参数(包括沉积电场，悬浮液浓度、组分的调节和搅拌状态)后，进行电泳共沉积。电泳沉积装置能很好的实现梯度功能陶瓷涂层的制备。具体过程是通过恒流泵和溢流作用使粉浆在电泳槽内自下而上流动，起到良好的搅拌、控制电泳液温度和调节电泳液成分的作用，可保证电泳槽内成分的连续变化。First, according to the performance requirements of the coating composite material to be prepared, optimize the coating composition and structure; then prepare the coating powder, screen the dispersion medium, and combine the analysis of the charging characteristics of the coating powder in the dispersion medium, surface modification. The present invention mainly uses bioactive glass (BG) particles and HA particles as coating raw materials to realize codeposition on the substrate (metal) as electrodes, and then determine process parameters (comprising deposition electric field, suspension) according to the deposition status of coating raw materials Concentration, adjustment of components and stirring state), electrophoretic co-deposition is carried out. The electrophoretic deposition device can well realize the preparation of functionally gradient ceramic coatings. The specific process is to make the slurry flow from bottom to top in the electrophoresis tank through the constant flow pump and overflow, which plays a good role in stirring, controlling the temperature of the electrophoresis liquid and adjusting the composition of the electrophoresis liquid, which can ensure the continuity of the components in the electrophoresis tank Variety.
根据涂层的梯度设计情况，将由内层占优的涂层原料(BG)制得的胶体悬浮液分散体系直接加入调节槽，其它涂层原料的胶体悬浮液分散体系由加液器加入，通过控制其加入的速度，即可按预先的设计连续改变电泳镀液的成分和实现梯度涂层。According to the gradient design of the coating, the colloidal suspension dispersion system made from the dominant coating material (BG) in the inner layer is directly added to the adjustment tank, and the colloidal suspension dispersion system of other coating materials is added from the liquid feeder, through By controlling the speed of its addition, the composition of the electrophoretic plating solution can be continuously changed and the gradient coating can be realized according to the pre-design.
最后，按确定的温度制度对涂层进行烧结处理(根据需要可选择采用大气氛中烧结、气氛保护烧结和真空烧结)，以强化涂层与基体的结合。Finally, the coating is sintered according to the determined temperature system (according to the needs, sintering in large atmosphere, atmosphere protection sintering and vacuum sintering can be selected) to strengthen the combination of coating and substrate.
本发明采用电泳共沉积工艺成功的研制了Ti6A14V/BG/HA的生物活性玻璃-陶瓷梯度涂层复合材料，涂层与基体的结合强度可达20MPa以上。主要技术工艺如下：1．涂层的设计The present invention successfully develops Ti6A14V/BG/HA bioactive glass-ceramic gradient coating composite material by adopting an electrophoretic co-deposition process, and the bonding strength between the coating and the substrate can reach more than 20 MPa. The main technical process is as follows: 1. coating design
首先研制了一种熔点较低，热膨胀系数与Ti6A14V相近的Na2O-CaO-SiO2-P2O5系统生物活性玻璃(BG)，作为Ti6A14V和羟基磷灰石(HA)间的高温粘结剂，通过BG和HA在涂层中的梯度分布，降低涂层的内应力，提高涂层的结合强度。其次，利用诱导HA在BG表面的结晶而制得由HA“包裹”的BG颗粒，改变BG颗粒表面的带电特性，实现了BG和HA在作为电极的Ti6A14V上的共沉积，以获得梯度涂层。2．涂层原料的制备Firstly, a bioactive glass (BG) of the Na 2 O-CaO-SiO 2 -P 2 O 5 system with a low melting point and a thermal expansion coefficient similar to that of Ti6A14V was developed as a high-temperature adhesive between Ti6A14V and hydroxyapatite (HA). The bonding agent, through the gradient distribution of BG and HA in the coating, reduces the internal stress of the coating and improves the bonding strength of the coating. Secondly, by inducing the crystallization of HA on the surface of BG to prepare BG particles "wrapped" by HA, changing the charging characteristics of the surface of BG particles, realizing the co-deposition of BG and HA on Ti6A14V as an electrode to obtain a gradient coating . 2. Preparation of Coating Raw Materials
将研制的生物玻璃熔融，经水碎和气流粉碎后，在无水乙醇中采用重力沉降分级的方法制取3μm以下的BG粉料，然后分散于0.005M的Ca(NO3)2中，向该悬浮液中滴加0.003M的(NH4)2HPO4和NH4OH，控制温度为40-50℃,pH=11-12，并不断搅拌，发生如下反应：The developed bioglass was melted, crushed by water and jet crushed, and the BG powder below 3 μm was prepared by gravity sedimentation and classification in absolute ethanol, and then dispersed in 0.005M Ca(NO 3 ) 2 to the Add 0.003M (NH 4 ) 2 HPO 4 and NH 4 OH dropwise to the suspension, control the temperature at 40-50°C, pH=11-12, and keep stirring, the following reaction occurs:
反应6小时后让其在该溶液中陈腐一周，除去表面漂浮物，然后过滤并用蒸馏水冲洗。干燥后加入无水乙醇球磨，即可制得已知粉浆浓度的胶体悬浮液。After 6 hours of reaction it was allowed to age in the solution for a week to remove superficial debris, then filtered and rinsed with distilled water. After drying, add absolute ethanol and ball mill to obtain a colloidal suspension with a known slurry concentration.
羟基磷灰石由复分解反应方法制得：将0.03M的(NH4)2HPO4逐滴滴加到0.05M的Ca(NO3)2中，并不断搅拌，保持pH=11-12,T=65℃，反应8h后，将母体溶液静置10天，除去表面漂浮物后，过滤、用蒸镏水冲洗，在真空干燥器中充分干燥后，再加入无水乙醇球磨，制得已知粉浆浓度的胶体悬浮液。3．电泳共沉积Hydroxyapatite is prepared by metathesis reaction: add 0.03M (NH 4 ) 2 HPO 4 dropwise to 0.05M Ca(NO 3 ) 2 and keep stirring to keep pH=11-12,T =65°C, after reacting for 8 hours, let the parent solution stand still for 10 days, remove the floating matter on the surface, filter, rinse with distilled water, fully dry in a vacuum desiccator, then add anhydrous ethanol and ball mill to obtain the known Colloidal suspension of slurry concentration. 3. electrophoretic co-deposition
将所制BG悬浮液和HA悬浮液经超声分散半小时后，分别加入调节槽和加液器中，开通磁力搅拌器和恒流泵；以经1500#SiC金相砂纸抛光、酸洗、丙酮超声清洗、重蒸镏水清洗、干燥后的Ti6A14V作为阴极，Pt为阳极，两极间距1cm，沉积电压为30V，待沉积30s后，通过分液漏斗向调节槽中添加HA悬浮液，调节好滴加速度，使在整个沉积过程中加入调节槽内的HA悬浮液的体积能与起初加入的BG悬浮液的体积相当。共沉积1-7min，待沉积完毕后，取出试样置于干燥器中干燥。4．烧结处理After ultrasonically dispersing the prepared BG suspension and HA suspension for half an hour, add them to the regulating tank and liquid feeder respectively, and turn on the magnetic stirrer and constant current pump; Ultrasonic cleaning, heavy distilled water cleaning, dried Ti6A14V was used as the cathode, Pt was used as the anode, the distance between the two electrodes was 1cm, and the deposition voltage was 30V. After 30s of deposition, add HA suspension to the adjustment tank through the separatory funnel to adjust the drop. Acceleration, so that the volume of HA suspension added to the conditioning tank during the entire deposition process can be equivalent to the volume of BG suspension added initially. Co-deposit for 1-7min. After the deposition is complete, take out the sample and place it in a desiccator to dry. 4. Sintering treatment
将已干燥的涂层试样置于管式炉中在氩气氛保护下进行烧结处理，处理温度为850℃-1000℃，保温1h，升温速度＜3℃/min，降温速度＜2℃/min。5．结果Put the dried coating sample in a tube furnace for sintering under the protection of argon atmosphere, the treatment temperature is 850°C-1000°C, keep it warm for 1h, the heating rate is less than 3°C/min, and the cooling rate is less than 2°C/min . 5. result
所制的HA改性BG粉所熔制的玻璃，其膨胀系数与Ti6A14V相匹配，是一种理想的涂层高温粘接材料，以其和HA为原料采用电泳沉积，可实现BG和HA的共沉积，经烧结，可获得Ti6A14V/BG/AH梯度涂层。采用的工艺参数为：沉积电压为30V，沉积时间为5min，在氩气氛保护下925℃对涂层进行烧结处理(保温1h)后，可得到最佳厚度约为50μm的涂层，涂层与基体的结合强度可达20MPa以上；用电子显微镜对其断面进行观察和分析，证明涂层是严格意义上的梯度涂层。The fused glass made of HA-modified BG powder has an expansion coefficient matching that of Ti6A14V, and is an ideal high-temperature bonding material for coatings. Using it and HA as raw materials by electrophoretic deposition can realize the combination of BG and HA. Co-deposition and sintering can obtain Ti6A14V/BG/AH gradient coating. The process parameters adopted are: the deposition voltage is 30V, the deposition time is 5min, and the coating is sintered at 925°C under the protection of argon atmosphere (1h of heat preservation), and the coating with an optimal thickness of about 50μm can be obtained. The bonding strength of the matrix can reach more than 20MPa; the observation and analysis of its cross-section with an electron microscope prove that the coating is a gradient coating in the strict sense.
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