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CHARACTERIZATION AND HYDRATION REACTIVITY OF α–TRICAICIUM PHOSPHATE PREPARED BY HEATING WITH GYPSUM 石膏加热法制备α -磷酸三钙的表征及水化反应性
Pub Date : 2012-01-01 DOI: 10.3363/PRB.27.1
H. Monma, Y. Moriyoshi, H. Ogata, T. Okura
Beta tricalcium phosphate (β-Ca3(PO4)2, β-TCP) mixed with gypsum (CaSO4・2H2O) was heated at 1300°C and 1400°C. The resulting products were characterized by DTA, XRD, FTIR, EDX and hydration reactivity. An inhibition effect on the transition of the low temperature form β to high temperature form α was observed with increasing the amount of gypsum. The substitution of SO4 for PO4 was suggested from increases of the β→α transition temperature and hydration reactivity. However both the substitution and the presence of S were not recognized by XRD, EDX and FTIR. Increasing the amount of gypsum resulted in the formation of hydroxyapatite (Ca5(OH)(PO4)3) at 1300°C and tetracalcium phosphate (Ca4(PO4)2O) at 1400°C. The hydration reactivity was in the order, pure α-TCP << α-TCP heated with gypsum. (Received Oct. 6, 2011; Accepted March 17, 2012)
将β-磷酸三钙(β-Ca3(PO4)2, β-TCP)与石膏(CaSO4·2H2O)混合在1300℃和1400℃下加热。通过DTA、XRD、FTIR、EDX和水化反应性对产物进行了表征。随着石膏用量的增加,对低温形态β向高温形态α的转变有抑制作用。β→α转变温度的升高和水化反应活性的提高表明SO4取代了PO4。但XRD、EDX和FTIR均未发现取代和S的存在。石膏添加量增加,在1300℃形成羟基磷灰石(Ca5(OH)(PO4)3),在1400℃形成磷酸四钙(Ca4(PO4)2O)。水化反应活性大小依次为纯α-TCP < α-TCP与石膏加热。(收于2011年10月6日;2012年3月17日录用)
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引用次数: 1
SURFACE PROPERTIES OF CERAMIC HYDROXYAPATITE ELECTRETS 陶瓷羟基磷灰石驻极体的表面性质
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.6
Katsuyuki Mukogawa, N. Wada, N. Horiuchi, Miho Nakamura, A. Nagai, T. Okura, K. Yamashita
: Hydroxyapatite (HAp) is the principal inorganic ingredient of human teeth and bone, and well-known as an excellent biocompatible material. HAp has been found to be polarized with an external electric field at a high temperature. Electrets are defined as the solids with functions that quasi-permanent surface charges. However, fundamental characteristics of electric fields due to HAp electrets have never been reported. Hence, this purpose is investigation of the properties of the surface electric fields of HAp bioceramic electrets; the surface potentials due to overlapping plural electrets with different electric potentials and signs; and a screening effect on electric fields with electrets due to a conductor and a dielectric. Polarized charges of the HAp electret have generated an electric field around the electret. The principle of superposition has held for the surface potentials of plural electrets. The screening effect by a conductor or a dielectric has been observed.
羟基磷灰石(HAp)是人类牙齿和骨骼的主要无机成分,是一种良好的生物相容性材料。在高温下发现HAp在外加电场作用下发生极化。驻极体被定义为具有准永久表面电荷函数的固体。然而,由HAp驻极体引起的电场的基本特性从未被报道过。因此,本研究的目的是研究HAp生物陶瓷驻极体的表面电场特性;具有不同电势和符号的复数驻极体重叠引起的表面电位;以及由于导体和电介质而产生的驻极体对电场的屏蔽效应。HAp驻极体的极化电荷在驻极体周围产生了电场。叠加原理适用于复数驻极体的表面电位。已经观察到导体或电介质的屏蔽效应。
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引用次数: 0
TECHNIQUES FOR PREPARING PURE β-TRICALCIUM PHOSPHATE GRANULES COMPOSED OF ROD-SHAPED PARTICLES 由棒状颗粒组成的纯β-磷酸三钙颗粒的制备技术
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.29
M. Kamitakahara, R. Fujii, K. Ioku
Hydrothermal, Phosphate Abstract: Spherical β-tricalcium phosphate (β-TCP) granules composed of rod-shaped particles are expected to be useful as bioresorbable bone substitutes. The β-TCP granules can be prepared by the heat treatment of Ca-deficient hydroxyapatite (HA) granules that are synthesized by hydrothermal treatment of  -TCP granules. However, when the Ca/P molar ratio of Ca-deficient HA becomes higher than 1.50, depending on the hydrothermal conditions, not only the β-TCP but also the HA phase appears following heat treatment. To resolve this problem, phosphate ions were incorporated into the Ca-deficient HA granules or monetite was added to decrease the Ca/P molar ratio to less than 1.50 in the starting composition. We revealed that these processes were effective in obtaining the pure  -TCP granules composed of rod-shaped particles and thus preventing
摘要:由棒状颗粒组成的球形β-磷酸三钙(β-TCP)颗粒有望成为生物可吸收的骨替代品。通过水热处理-TCP颗粒合成的缺钙羟基磷灰石(HA)颗粒,可以制备β-TCP颗粒。然而,当Ca/P摩尔比大于1.50时,根据水热条件的不同,热处理后不仅出现β-TCP相,还出现HA相。为了解决这一问题,在缺乏钙的HA颗粒中加入磷酸根离子或在起始成分中加入钱铁矿,使Ca/P摩尔比降低到1.50以下。我们发现,这些工艺可以有效地获得由棒状颗粒组成的纯-TCP颗粒,从而防止
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引用次数: 1
IN VITRO BIORESORBABILITY OF CHELATE-SETTING CEMENTS WITH VARIOUS CALCIUM-PHOSPHATE PHASES 不同钙-磷酸相螯合固结物的体外生物可吸收性
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.105
H. Manabe, Toshiisa Konishi, Minori Mizumoto, M. Honda, M. Aizawa
: We have developed calcium-phosphate cement (CPC) that can be formed into any desired shapes during an operation. The novel hydroxyapatite (HAp) and tricalcium phosphate (TCP) cements set on the basis of chelate-bonding ability of inositol phosphate (IP6). In the present study, we evaluated dissolution rate of various CPCs under conditions of acetic acid buffer solution at pH5.5. The concentration of calcium ions released from the CPCs with HAp,  -TCP and  -TCP phases in the acetic acid buffer solution was continuously measured using a calcium ion meter. The dissolution rate of samples decreased in order of  -TCP >  -TCP > HAp derived from wet process
我们已经开发出磷酸钙水泥(CPC),它可以在手术过程中形成任何所需的形状。新型羟基磷灰石(HAp)和磷酸三钙(TCP)胶结物是基于磷酸肌醇(IP6)的螯合能力而形成的。在本研究中,我们在pH5.5的醋酸缓冲溶液中测定了各种CPCs的溶出率。用钙离子计连续测定醋酸缓冲液中HAp、-TCP和-TCP相cpc释放的钙离子浓度。湿法制得的样品溶解速率依次为-TCP >-TCP > HAp
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引用次数: 2
BEYOND CURRENT INTERPRETATION OF BONDING BETWEEN SILICATE CERAMICS AND BONE 超出了目前硅酸盐陶瓷和骨骼之间的结合的解释
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.18
A. Osaka
: The formation of strong bond between material and bone tissue, studied by Hench, Kokubo, Yamamuro, or others in 1980's is revisited to obtain some insight into apatite deposition on meso- or microporous silica gel, derived by phase separation in the system tetraethoxysilane, polyethylene glycol, and water. Testing the apatite-depositing ability on the silica gels indicated that the increase in calcium, phosphate, and hydroxyl ions in Kokubo's simulated body fluid differently affected the apatite nucleation rate, and suggested necessity of modifying the original simplistic model of apatite nucleation: calcium ion adsorption triggered nucleation. Apatite formation was reviewed on anatase layer prepared on Ti due to chemical (H 2 O 2 ) and heating treatments (CHT procedure), and balanced clustering of calcium and phosphate ions is significant for the apatite nucleation. CHT layer is proposed as a reference material for bone-bonding testing.
Hench, Kokubo, Yamamuro等人在20世纪80年代研究的材料与骨组织之间强键的形成,重新审视了磷灰石沉积在中孔或微孔硅胶上的一些见解,通过在四乙氧基硅烷,聚乙二醇和水的体系中进行相分离而得到。对硅胶的磷灰石沉积能力的测试表明,Kokubo模拟体液中钙离子、磷酸盐离子和羟基离子的增加对磷灰石成核速率的影响不同,表明有必要修改原来的磷灰石成核简单模型:钙离子吸附触发成核。本文综述了钛表面经过化学(h2o2)和加热(CHT)处理制备的锐钛矿层中磷灰石的形成过程,指出钙离子和磷酸盐离子的平衡聚集对磷灰石成核具有重要意义。建议将CHT层作为骨结合测试的参考材料。
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引用次数: 1
SINTERING AND OSTEOCLAST BEHAVIOR OF CARBONATE APATITE CERAMICS 碳酸盐磷灰石陶瓷的烧结及破骨行为
Pub Date : 2012-01-01 DOI: 10.3363/PRB.27.45
Takanori Watarai, Miho Nakamura, N. Horiuchi, K. Hashimoto, A. Nagai, K. Yamashita
B-type carbonate apatite (CA) substituting for phosphate ions, is the major inorganic components of vertebrate bones. CA is more biodegradable than HA and has been expected as a next generation biomaterial. We had reported that the polarized HA could promote bone healing. The purpose of this study was to investigate the effects of the electrically polarization on CA characterization. CA synthesized by wet method was sintered at various temperatures in carbon dioxide atmosphere. The TG measurement and polarization treatment of the sintered CA were performed. From the results of XRD and FT-IR analyses, CA was inclusion of contain carbonate about 5wt%. From TSDC measurement, the quantity of accumulated charges of CA was larger than HA. In addition, we evaluated the osteoclast behaviors on non-polarized CA and polarized CA. From the observation of cell morphology, there were multinucleated cells having actin ring structures specific for the activated osteoclasts on the CA surfaces. (Received May 7 2012; Accepted August 6, 2012)
b型碳酸盐磷灰石(CA)取代磷酸盐离子,是脊椎动物骨骼的主要无机成分。CA比HA更易生物降解,有望成为下一代生物材料。我们曾报道过极化的HA能促进骨愈合。本研究的目的是探讨电极化对CA表征的影响。用湿法合成的CA在不同温度下在二氧化碳气氛中烧结。对烧结后的CA进行了热重测定和极化处理。XRD和FT-IR分析表明,CA中含有约5wt%的含碳酸盐。从TSDC测量来看,CA的累积电荷量大于HA。此外,我们还评估了非极化CA和极化CA上的破骨细胞行为。从细胞形态观察,CA表面存在具有活化破骨细胞特异性肌动蛋白环结构的多核细胞。(2012年5月7日收稿;2012年8月6日接受)
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引用次数: 0
RECOVERY AND ENRICHMENT OF AQUEOUS PHOSPHATE FROM THE SLAG RELEASED BY A CHEMICAL FACTORY 从化工厂排放的矿渣中回收和富集含水磷酸盐
Pub Date : 2012-01-01 DOI: 10.3363/PRB.27.23
S. Sugiyama, Tomoki Hayashi, Ippei Shinomiya, Keizo Nakagawa, K. Sotowa
The elution behaviors of phosphate from the slag released by a chemical factory using various eluates were examined. Since this slag was covered with organic species, two pretreatment methods for the slag one the calcination of the slag and the other the trituration of the slag were employed to strip away the organic species from the slag. Since the elution rate from the pre-triturated slag was evidently greater than that from the pre-calcined slag, the elution behavior of the former was mainly examined in the present study. For the efficient elution of phosphate from the slag, the use of 1M HNO3 as an eluate and 30 min of trituration time were suitable. Unfortunately, together with the elution of phosphate from the slag, some cationic species were simultaneously eluted. In the present study, the removal behavior of iron cation, which was a main contaminant in the slag, using calcium hydroxyapatite (CaHAp) was also examined. Even when the solution obtained by the elution of the slag was employed for the removal of Fe using CaHAp, the Fe could be favorably removed from the solution. Results from the present study suggests that unused phosphate in slag is a potential source of raw material for rare
研究了不同洗脱液对某化工厂废渣中磷酸盐的洗脱行为。由于该矿渣被有机物质所覆盖,采用烧渣和磨渣两种预处理方法去除矿渣中的有机物质。由于预焙烧渣的洗脱速率明显大于预焙烧渣的洗脱速率,因此本文主要研究预焙烧渣的洗脱行为。为有效洗脱矿渣中的磷酸盐,以1M HNO3为洗脱剂,加盐时间为30 min为宜。不幸的是,在从矿渣中洗脱磷酸盐的同时,也同时洗脱了一些阳离子。本文还研究了羟基磷灰石钙(CaHAp)对矿渣中主要污染物铁阳离子的去除行为。即使将渣洗脱得到的溶液用于CaHAp除铁,也能很好地将铁从溶液中去除。研究结果表明,矿渣中未使用的磷酸盐是稀土原料的潜在来源
{"title":"RECOVERY AND ENRICHMENT OF AQUEOUS PHOSPHATE FROM THE SLAG RELEASED BY A CHEMICAL FACTORY","authors":"S. Sugiyama, Tomoki Hayashi, Ippei Shinomiya, Keizo Nakagawa, K. Sotowa","doi":"10.3363/PRB.27.23","DOIUrl":"https://doi.org/10.3363/PRB.27.23","url":null,"abstract":"The elution behaviors of phosphate from the slag released by a chemical factory using various eluates were examined. Since this slag was covered with organic species, two pretreatment methods for the slag one the calcination of the slag and the other the trituration of the slag were employed to strip away the organic species from the slag. Since the elution rate from the pre-triturated slag was evidently greater than that from the pre-calcined slag, the elution behavior of the former was mainly examined in the present study. For the efficient elution of phosphate from the slag, the use of 1M HNO3 as an eluate and 30 min of trituration time were suitable. Unfortunately, together with the elution of phosphate from the slag, some cationic species were simultaneously eluted. In the present study, the removal behavior of iron cation, which was a main contaminant in the slag, using calcium hydroxyapatite (CaHAp) was also examined. Even when the solution obtained by the elution of the slag was employed for the removal of Fe using CaHAp, the Fe could be favorably removed from the solution. Results from the present study suggests that unused phosphate in slag is a potential source of raw material for rare","PeriodicalId":20022,"journal":{"name":"Phosphorus Research Bulletin","volume":"389 1","pages":"23-27"},"PeriodicalIF":0.0,"publicationDate":"2012-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79716739","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 8
FABRICATION AND EVALUATION OF SILICON-CONTAINING APATITE FIBER SCAFFOLDS FOR BONE TISSUE ENGINEERING 骨组织工程用含硅磷灰石纤维支架的制备与评价
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.101
Y. Kinoshita, S. Best, M. Aizawa
The aim of this work is to develop a highly-functional tissue engineering scaffold from silicon-containing apatite fibres (Si-AF). Firstly, Si-AFs were synthesized by a homogeneous precipitation method. Starting solution with a Ca/(P+Si) ratio of 1.67 was prepared by mixing Ca(NO3)24H2O, (NH4)2HPO4, Si(OC2H5)4 (TEOS), (NH2)2CO and HNO3. The concentrations of TEOS in the starting solution were 0 (AF), 0.8 (0.8Si-AF) and 1.6 (1.6Si-AF) mass%. Next, Si-AF scaffolds (Si-AFS) were fabricated by firing the compacts consisting of Si-AF and carbon beads of 150 m diameter. The resulting Si-AFSs were characterized using X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Results showed that the material properties of the 0.8Si-AFS were similar to those of the conventional AFS without silicon. Consequently, we can conclude that the 0.8Si-AFS offers as a potential novel scaffold material, creating a three-dimensional cell culture environment. (Received March 29, 2012; Accepted April 9, 2012)
这项工作的目的是从含硅磷灰石纤维(Si-AF)中开发一种高功能的组织工程支架。首先,采用均匀沉淀法合成了Si-AFs。将Ca(NO3)2、(NH4)2HPO4、Si(OC2H5)4 (TEOS)、(NH2)2CO和HNO3混合,制得Ca/(P+Si)比为1.67的起始溶液。起始溶液中TEOS的浓度分别为0 (AF)、0.8 (0.8 si -AF)和1.6 (1.6 si -AF)质量%。接下来,通过烧制由Si-AF和直径为150m的碳珠组成的致密物,制备Si-AF支架(Si-AFS)。采用x射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、扫描电镜(SEM)和电感耦合等离子体原子发射光谱(ICP-AES)对所得的Si-AFSs进行了表征。结果表明,0.8Si-AFS的材料性能与常规无硅AFS相似。因此,我们可以得出结论,0.8Si-AFS作为一种潜在的新型支架材料,可以创建三维细胞培养环境。(2012年3月29日收稿;2012年4月9日接受)
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引用次数: 2
PHOSPHATE GLASSES AND GLASS-CERAMICS FOR BIOMEDICAL APPLICATIONS 生物医学应用的磷酸盐玻璃和玻璃陶瓷
Pub Date : 2012-01-01 DOI: 10.3363/PRB.26.8
T. Kasuga, T. Hattori, M. Niinomi
Calcium phosphate glasses and glass-ceramics with some limited compositions show bioactivity. The glasses could be prepared by including a small amount of TiO2 and/or Na2O: the typical compositions were 60CaO-30P2O5-xTiO2-(10‒ x)Na2O in mol%. The glasses include orthophosphate and pyrophosphate groups. Hydroxyapatite (HA) forming ability in a simulated body fluid (SBF) is often examined to know the chemical properties of materials for biomedical applications. On the 60CaO-30P2O5-xTiO2-(10‒x)Na2O glasses, HA formed within 7-10 days. In the case of the glasses, the HA-forming ability is suggested to be influenced by various factors such as the basicity of a gel layer formed on them in SBF and the amount of the functional groups for HA nucleation in the layer. Modification of the glass composition, which MgO was substituted to CaO, improved the glassification tendency of the glasses due to the high field strength of Mg. The MgO-containing glass included a larger amount of orthophosphate group than the original glass, and showed higher ion-releasing ability. Bivalent ions in the phosphate invert glasses play an important role in their glassification and ion-releasing. The glasses were crystallized and subsequently sintered by heating their powder-compacts. The resulting glass-ceramics consist of -Ca3(PO4)2 and -Ca2P2O7 with residual glassy phase. Their HA-forming ability in SBF was enhanced after autoclaving in distilled water. By the autoclaving, sodium, calcium, phosphate ions in the glassy phase around the surface dissolved and anatase crystals formed. The glass-ceramics could be coated strongly on a new -type titanium alloy using a conventional glazing technique. The glass-ceramic-coated materials were implanted into the femurs of Japanese rabbits. After 1 month, bone tissue contacted directly with the coating. After 5 years of implantation, the coating was clarified to be work as a bioactive material on the titanium alloy. (Received January 27, 2012; Accepted February 16, 2012)
磷酸钙玻璃和微晶玻璃具有一定的生物活性。通过加入少量TiO2和/或Na2O可以制备玻璃:典型的组成为60CaO-30P2O5-xTiO2-(10 -x)Na2O(摩尔%)。玻璃包括正磷酸盐和焦磷酸盐基团。羟基磷灰石(HA)在模拟体液(SBF)中的形成能力经常被检测,以了解生物医学应用材料的化学性质。在60CaO-30P2O5-xTiO2-(10-x)Na2O玻璃上,HA在7-10天内形成。在玻璃的情况下,HA的形成能力被认为受到各种因素的影响,如在SBF中形成的凝胶层的碱度和层中HA成核的官能团的数量。用氧化镁代替CaO对玻璃组分进行改性,由于Mg的高场强,使玻璃的玻璃化倾向得到改善。含氧化镁玻璃比原玻璃含有更多的正磷酸盐基团,并表现出更高的离子释放能力。磷酸反晶玻璃中的二价离子在其玻璃化和离子释放中起着重要作用。玻璃被结晶,然后通过加热它们的粉末压坯烧结。所得微晶玻璃由-Ca3(PO4)2和-Ca2P2O7组成,并伴有残余玻璃相。经蒸馏水高压灭菌后,其在SBF中的ha形成能力增强。通过高压灭菌,钠、钙、磷酸盐离子在玻璃相表面周围溶解,形成锐钛矿晶体。使用传统的上釉技术,玻璃陶瓷可以被牢固地涂在一种新型型钛合金上。将玻璃陶瓷包覆材料植入日本家兔股骨。1个月后,骨组织与涂层直接接触。经过5年的植入,涂层可以作为生物活性材料在钛合金上发挥作用。(2012年1月27日收稿;2012年2月16日接受)
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引用次数: 23
EFFECT OF β-CALCIUM ORTHOPHOSPHATE ADDITION ON HIGH- TEMPERATURE PLASTIC DEFORMATION OF HYDROXYAPATITE WITH SUBMICROMETER-SIZED GRAINS 添加β-正磷酸钙对亚微米颗粒羟基磷灰石高温塑性变形的影响
Pub Date : 2012-01-01 DOI: 10.3363/PRB.27.11
Y. Asano, Y. Sakka, J. DaviesIan, S. Koda, K. Itatani
The effect of -calcium orthophosphate (-Ca3(PO4)2:-TCP) addition (1 ~ 20 mass%) on the high-temperature plastic deformation of hydroxyapatite (Ca10(PO4)6(OH)2:HAp) ceramic specimen was examined. The high-density HAp ceramic body with -TCP addition, which was composed of submicrometer-sized grains, was fabricated by pulse-current pressure firing at a temperature between 900 and 1050C for 10 min under a pressure of 50 MPa. The relative densities of HAp ceramics with 1 to 20 mass% -TCP addition fabricated by pulse-current pressure firing at 1000C for 10 min exceeded 99%; the grain sizes increased from 0.2 to 0.3 m with increasing -TCP addition from 0 to 10 mass% and then steeply to 0.9 m with increasing -TCP addition from 10 to 20 mass%. The tensile strain of the HAp specimen with 1 mass% -TCP addition pulse-current pressure fired at 1000C for 10 min achieved a maximum of 390% for a test temperature of 1000C and a strain rate of 1.48  10 -4 s -1 , compared to 364% for the monolithic HAp specimen.
研究了-正磷酸钙(-Ca3(PO4)2:-TCP)添加量(质量% 1 ~ 20%)对羟基磷灰石(Ca10(PO4)6(OH)2:HAp)陶瓷试样高温塑性变形的影响。采用脉冲电流加压烧制工艺,在温度900 ~ 1050℃范围内,在50 MPa压力下,制备了含有-TCP的亚微米级高密度HAp陶瓷体。添加1 ~ 20质量%-TCP的脉冲电流压力在1000℃下烧制10 min,制备的HAp陶瓷相对密度超过99%;当-TCP添加量从0到10质量%时,晶粒尺寸从0.2增大到0.3m;当-TCP添加量从10到20质量%时,晶粒尺寸急剧增大到0.9m。在质量为1 %-TCP的脉冲电流压力下,在1000颈椎颈椎下持续10分钟的拉伸应变在1000颈椎颈椎温度下达到了最大的390%,应变率为1.4810 -4 s -1,而整体HAp试件的应变率为364%。
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引用次数: 0
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Phosphorus Research Bulletin
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