烧结温度对3D打印硅基陶瓷型芯表面形貌及粗糙度的影响

单晶高温合金空心叶片是航空发动机的重要部件, 其内腔结构是采用陶瓷型芯制备的。随着航空发动机推重比提高, 型芯结构越来越复杂, 传统制备工艺受限, 光固化3D打印陶瓷型芯技术为复杂结构型芯的制备提供了一种可行方案。为了改善光固化3D打印陶瓷型芯因台阶效应导致的表面粗糙度较大的问题, 本研究利用固含量体积分数63%的硅基型芯浆料进行光固化3D打印型芯, 并在1100~1300 ℃对型芯素坯进行烧结, 对烧成的硅基陶瓷型芯的微观结构、元素分布、相组成、型芯打印面和打印堆积方向的表面形貌和粗糙度进行分析。研究发现型芯打印面平整, 无明显表面缺陷, 1100、1200和1300 ℃烧结型芯的打印面粗糙度分别为1.83、1.24和1.44 μm; 片层堆积方向的表面有片层结构特征, 片层间出现微裂纹, 1200 ℃以上烧结的型芯表面粗糙度达到空心叶片使用要求(R_a≤2.0 μm)。结果表明不同烧结温度会改变型芯烧结过程中的液相含量、莫来石生成量、莫来石生成形态和颗粒间玻璃相的分布, 从而对光固化3D打印硅基陶瓷型芯的表面粗糙度产生明显影响。光固化3D打印陶瓷型芯技术结合烧结工艺能制备出满足先进空心叶片用硅基陶瓷型芯表面要求的粗糙度。     

覆膜不锈钢粉末选择性激光烧结成型机理研究

制备了一种适合于选择性激光烧结快速成型技术的覆膜不锈钢(1Cr18Ni9Ti)粉末材料,应用激光烧结快速成型机对自行开发的覆膜不锈钢粉末进行了烧结成型实验.应用微观分析方法研究了覆膜不锈钢粉末激光烧结成型动态过程,在此基础上建立了覆膜不锈钢粉末的激光烧结成型过程机理模型,当加热温度100℃＜T＜130℃时,粘性流动为主要的成型机理;当加热温度T＞130℃时,可以用熔化/固化机理来描述.     

用丝网印刷法制备Pt电极及其性能

采用单层和双层印刷法在氧化铝衬底上制备功能陶瓷厚膜用Pt电极,研究了烧结温度、升温速率和电极厚度对Pt电极层的表面形貌、表面覆盖率和表面粗糙度的影响,以揭示晶粒长大、气孔生长及致密化机制.结果表明,在单层印刷Pt电极的烧结过程中,低温阶段残留的碳使不同温区Pt的主导扩散机制不同.双层印刷Pt电极中第一层在600℃下烧结后,印刷第二层再在1200℃下烧结具有最大表面覆盖率和最小平均粗糙度(其值约为0.82 μm),同时具有最好的导电性能(方阻为0.044 Ω/□).     

Fabrication and sintering of Pt electrode deposited by screen printing method

采用单层和双层印刷法在氧化铝衬底上制备功能陶瓷厚膜用Pt电极, 研究了烧结温度、升温速率和电极厚度对Pt电极层的表面形貌、表面覆盖率和表面粗糙度的影响,以揭示晶粒长大、气孔生长及致密化机制. 结果表明, 在单层印刷Pt电极的烧结过程中,低温阶段残留的碳使不同温区Pt的主导扩散机制不同.双层印刷Pt电极中第一层在600℃下烧结后,印刷第二层再在1200℃下烧结具有最大表面覆盖率和最小平均粗糙度(其值约为0.82 um),同时具有最好的导电性能(方阻为0.044 Ω/□).     

金矿尾矿制备烧结砖的力学性能

本研究以金矿尾矿为主料,黏土为辅料制备烧结砖,探究原料配比、成型水分及烧制工艺对尾矿烧结砖抗压强度、吸水率,体积密度和烧失重的影响.结果显示:烧结砖的抗压强度、烧失重和体积密度随黏土掺量、烧结时间和保温时间的增加而增大;吸水率随黏土掺量、烧结时间和保温时间的增加而减小;烧结砖吸水率、烧失重和体积密度随成型水分的增加而增大.在尽量利用金矿尾矿的前提下,制备的金矿尾矿烧结砖的最佳烧制参数为:金矿尾矿:黏土(质量比)为7:3、成型水分25％、烧结温度1000℃、保温时间2 h.在砖烧制过程中,随温度升高,砖坯中结合水、结构水及结晶水随之排出;原料中透长石、硫铁矿、蒙脱石和方解石发生分解,形成了赤铁矿和钙长石.     

泡沫碳化硅细胞相容性及动物体内植入实验研究

采用高分子热解结合可控熔渗反应烧结方法制备泡沫SiC,观察体外接种到泡沫SiC表面的成骨细胞MG63的贴壁和生长状况,评价泡沫SiC的细胞相容性.通过建立兔下颌临界骨缺损人工材料植入模型,进行大体标本观察、组织学观察及图像分析,探讨了泡沫SiC作为骨替代材料的可行性.研究结果表明,体外成骨细胞MG63在泡沫SiC表面的生长状态良好.体内植入实验的26只实验动物健康状况良好,伤口均为一期愈合.大体标本观察表明,各时间点内的泡沫SiC周边及其内部网孔内均有不同程度的骨组织形成;组织学观察可见骨组织的修复属于正常的骨修复过程.植入4w后,泡沫SiC内新生骨的四环素荧光标记率和成骨面积均低于HA,而在8w及24w后与HA接近,其差异无统计学意义.由此表明泡沫SiC具有良好的细胞相容性,且泡沫SiC修复兔下颌骨缺损的远期效果与HA相似,具有较好的骨传导性.     

燃烧法合成铪酸钇粉体及其透明陶瓷的制备

以硝酸钇(Y(NO₃)₃)和氯化铪(HfCl₄)为原料, 乙二胺四乙酸(EDTA)作为燃剂, 采用燃烧法制备了粒径为50nm左右的纯相铪酸钇粉体. 粉体经1200℃煅烧后高能球磨15h, 然后在200MPa条件下进行冷等静压成型, 素坯尺寸为20mm×2.5mm, 最后采用真空烧结(1850℃保温6h), 制备出可见光波段直线透过率为50%的铪酸钇透明陶瓷. 研究了真空烧结温度对样品透过率和显微结构的影响, 当烧结温度高于1850℃时, 温度对于透过率影响不是很明显; 随着烧结温度的升高, 样品的晶粒尺寸增大.     

金刚石表面形成Ti3SiC2的反应机理

采用Ti、Si、TiC、金刚石磨料为原料,通过放电等离子烧结(SPS),制备了Ti3SiC2陶瓷结合剂金刚石材料.研究结果表明,Ti-Si-2TiC试样经SPS加热的过程中位移、位移率和真空度在1200℃时发生明显变化,表明试样发生了物理化学变化.XRD分析结果表明1200℃时试样发生化学反应生成了Ti3SiC2.随着温度升高,试样中Ti3SiC2含量逐渐增加.当烧结温度为1200℃、1300℃、1400℃和1500℃时,产物中Ti3SiC2含量分别为65.9%、79.97%、87.5%和90.1%.在Ti/Si/2TiC粉料中添加适量的金刚石5%和10%进行烧结,并未抑制Ti3SiC2的反应合成.SEM观察表明,金刚石与基体结合紧密,同时其表面生长着发育良好的Ti3SiC2板条状晶粒.提出了一种金刚石表面形成Ti3SiC2的机制,即金刚石表面的碳原子首先与周围的Ti反应生成TiC,然后TiC再与Ti-Si相发生化学反应,生成Ti3SiC2.     

SDC电解质致密化研究

以共沉淀-喷雾干燥法制备的Ce0.8 Sm0.2 O1.9(SDC)粉体为原料,模压成型后高温烧结获得SDC电解质陶瓷片.研究模压成型过程中加压时间、压力大小以及烧结温度对烧结体致密度的影响,利用XRD和SEM分别对不同烧结温度获得的烧结体结构和表面形貌进行分析.研究表明,压力30MPa、加压时间30min后获得的坯体,随着烧结温度的升高,烧结体致密度呈上升趋势,烧结温度达到1450℃时进入烧结后期,烧结体具有较高的致密度.此外,通过测定烧结过程中坯体收缩率,对SDC电解质陶瓷片的烧结动力学进行了研究,从而确定SDC电解质致密化的烧结温度为1300～1500℃.     

HAp/SiO2复合陶瓷材料的制备及体外生物活性

HAp和SiO2的混合粉末压制成型后,在1200℃下烧结得到含5.0%(质量分数)SiO2的HAp/SiO2生物陶瓷复合材料。烧结体的XRD及FT-IR分析结果表明,SiO2的添加促进了HAp发生热分解。其主要物相为α-TCP、HAp、Ca2P2O7以及生物玻璃(bioglass,BG)等。体外生物活性实验结果显示,样品浸泡在模拟体液(SBF)中24h后,表面出现花瓣状磷灰石沉积物,72h后进而生成板状沉积物,120h后在样品表面覆盖了较厚的类骨磷灰石层,经XRD测试分析表明,该层主要为碳酸羟基磷灰石(HCA)。制备的HAp-5.0%(质量分数)SiO2生物陶瓷复合材料具有比纯HAp更加优越的体外生物活性,可期待作为一种新的骨修复材料。     

Polyetheretherketone and titanium surface treatments to modify roughness and wettability-Improvement of bioactivity and antibacterial properties

Among the materials available for implant production,titanium is the most used while polyetherether-ketone (PEEK) is emerging thanks to its stability and to the mechanical properties similar to the ones of the bone tissue.Material surface properties like roughness and wettability play a paramount role in cell adhesion,cell proliferation,osteointegration and implant stability.Moreover,the bacterial adhesion to the biomaterial and the biofilm formation depend on surface smoothness and hydrophobicity.In this work,two different treatments,sandblasting and air plasma,were used to increase respectively roughness and wettability of two materials:titanium and PEEK.Their effects were analyzed with profilometry and contact angle measurements.The biological properties of the material surfaces were also investigated in terms of cell adhesion and proliferation of NIH-3T3 cells,MG63 cells and human Dental Pulp Stem Cells.Moreover,the ability of Staphylococcus aureus to adhere and form a viable biofilm on the samples was evaluated.The biological properties of both treatments and both materials were compared with samples of Synthegra(R) titanium,which underwent laser ablation to obtain a porous micropatterning,character-ized by a smooth surface to discourage bacterial adhesion.All cell types used were able to adhere and proliferate on samples of the tested materials.Cell adhesion was higher on sandblasted PEEK samples for both MG63 and NIH-3T3 cell lines,on the contrary,the highest proliferation rate was observed on sandblasted titanium and was only slightly dependent on wettability;hDPSCs were able to proliferate similarly on sandblasted samples of both tested materials.The highest osteoblast differentiation was ob-served on laser micropatterned titanium samples,but similar effects,even if limited,were also observed on both sandblasted materials and air plasma treated titanium.The lowest bacterial adhesion and biofilm formation was observed on micropatterned titanium samples whereas,the highest biofilm formation was detected on sandblasted PEEK samples,and in particular on samples not treated with air-plasma,which displayed the highest hydrophobicity.The results of this work showed that all the tested materials were able to sustain osteoblast adhesion and promote cell proliferation;moreover,this work highlights the fea-sible PEEK treatments which allow to obtain surface properties similar to those of titanium.The results here reported,clearly show that cell behavior depends on a complex combination of surface properties like wettability and roughness and material nature,and while a rough surface is optimal for cell adhesion,a smooth and less hydrophilic surface is the best choice to limit bacterial adhesion and biofilm formation.     

陶瓷微结构件的注射成形工艺及其微观组织

采用粉末微注射成形技术制作了ZrO2陶瓷微结构件,分析了其注射成形工艺,包括喂料配制、注射工艺及烧结工艺对微观组织的影响.实验结果表明,粉末体积分数为55%的生坯注射成形后在1 500℃下烧结2 h,采用排水法测得其微结构相对密度高达98.5%,采用纳米硬度分析法得到其微结构的显微硬度值为13.75 GPa.扫描电子显微镜(SEM)结果表明,提高模具温度和注射压力,有利于微结构的填充,进而改善微结构件的微观组织;高的烧结温度可以增加零件的致密度,但容易导致晶粒的过度长大和尺寸不均匀.激光共聚焦光学显微镜观察结果表明,使用亚微米级陶瓷超细粉得到的微结构具有良好的表面质量,其烧结前、后的表面粗糙度值分别为0.33μm和0.28μm.此外,提高粉末含量可以减小零件收缩率,从而有利于微结构的尺寸精度控制.     

羟基磷灰石-钛酸钡仿人骨复合材料的制备及其性能

以HA粉和BT粉为原料,用烧结工艺制备羟基磷灰石-钛酸钡(HA-BT)仿人骨复合材料,使用D/max2200PCX光衍射仪、S4800场发射扫描电镜及其附带的X射线能谱仪、STA449F3同步热分析仪、1036PC万能材料试验机、LC2735准静态压电系数测量仪和ZJD-C型介电常数测试仪对其表征,研究BT含量和烧结温...     

Evaluation of the attachment,proliferation, and differentiation of osteoblast on a calcium carbonate coating on titanium surface

Titanium has been reported to have some limitations in dental and orthopaedic clinical application. This study described a coating process using a simple chemical method to prepare calcium carbonate coatings on smooth titanium (STi) and sandblasted and acid-etched titanium (SATi), and evaluated the biological response of the materials in vitro. The surfaces of STi, SATi, calcium carbonate coated STi (CC-STi) and calcium carbonate coated SATi (CC-SATi) were characterized for surface roughness, contact angles, surface morphology and surface chemistry. The morphology of MG63 cells cultured on the surfaces was observed by SEM and Immuno-fluorescence staining. Cell attachment/proliferation was assessed by MTT assay, and cell differentiation was evaluated by alkaline phosphatase (ALP) activity. MG63 was found to attach favorably to calcium carbonate crystals with longer cytoplasmic extensions on CC-STi and CC-SATi, resulting in lower cell proliferation but higher ALP activity when compared to STi and SATi respectively. Moreover, CC-SATi is more favorable than CC-STi in terms of biological response. In conclusion, the calcium carbonate coatings on titanium were supposed to improve the osteointegration process and stimulate osteoblast differentiation, especially in early stage. And this method could possibly be a feasible alternative option for future clinical application.     

直接凝固注模成型氮化硅陶瓷

直接凝固注模成型是一种新颖的原位凝固成型工艺,特别适合于复杂形状陶瓷部件的成型．通过粉体的表面改性、浆料ｐＨ值的调节以及引入高效分散剂等途径制备出了低粘度高固含量的氮化硅浆料,通过直接凝固注模成型可以获得适当的素坯密度和强度．坯体气孔分布均匀,为较窄的单峰分布,断口光滑平整,坯体各部位密度具有很好的均匀性．在相对较低的烧结温度下（１７５０℃）,成型坯体经过无压烧结可达到理论密度的９８％,基本实现致密化．烧结体结构均匀,晶粒均匀生长,发育良好．经１８００℃烧结２ｈ后,抗折强度达７５８．４ ＭＰａ,断裂韧性为６．３ＭＰａ·ｍ^１／２．     

Initial Attatchment of rMSC and MG‐63 Cells on Patterned Bioglass® Substrates

A soft lithography technique was used to introduce surface patterns on the surface of sintered bioactive glass substrates. Osteoblast‐like MG‐63 cells and rat mesenchymal stem cells (rMSC) seeded on micropatterned bioactive glass surfaces showed different behavior with rMSC exhibiting a better initial attachment than MG‐63 cells. Both cytoskeleton formation and cell spreading of rMSC were supported by the bioactive surfaces. In addition, the structured surfaces seemed to guide MG‐63 cells to a larger extent than rMSC. The in vitro results are important considering the continuous development of bone tissue scaffolds based on silicate bioactive glasses.     

金属粉末注射成形钛合金工艺研究

为了探究保障最终产品性能满足ASTM标准的粉末注射成形工艺,本文采用金属粉末注射成形方法,以德国Basf公司提供的喂料为原料,通过对注射参数优化获取1组最优注射工艺参数,用于后续脱脂及烧结工艺.利用拉伸、弯曲等力学实验,扫描电镜、金相光学显微镜等表征方法对材料的力学性能及微观结构进行表征,研究了注射、脱脂和烧结工艺参数...     

Effect of anodization on corrosion behaviour and biocompatibility of Cp-titanium in simulated body fluid

The objective of this investigation is to study the effectiveness of anodized surface of commercial purity titanium (Cp-Ti) on its corrosion behaviour in simulated body fluid (SBF) and proliferation of osteoblast cells on it, to assess its potentiality as a process of surface modification in enhancing corrosion resistance and osseointegration of dental implants. Highly ordered nano-porous oxide layer, with nano-sized pores, is developed on the surface of Cp-Ti through electrochemical anodization in the electrolyte of aqueous solution of 0·5% HF at 15 V for 30 min at 24 °C. The nano-porous feature of the anodized surface is characterized by field-emission scanning electron microscope (FESEM). Pores of some anodized samples are sealed by exposing the anodized surface in boiling water. Corrosion behaviour of the anodized specimen is studied in Ringer’s solution at 30 ± 2 °C, using electrochemical impedance and cyclic polarization technique. Biocompatibility of the anodized surface is accessed using MG63 osteoblast cells. Both corrosion as well as pitting resistance of Cp-Ti in simulated body fluid are found to be highest in the anodized and sealed condition and followed in decreasing order by those of anodized and unanodized ones. Significantly higher MG63 osteoblast cell proliferations are found on the anodized surface than that on the unanodized one. Anodized Cp-Ti develops nano-size surface pores, like that of natural bone. It enhances corrosion and pitting resistance and also the process of osteoblast cell proliferation on Cp-Ti.