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CN118184332A - Hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial and preparation method thereof - Google Patents

Hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial and preparation method thereof Download PDF

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Publication number
CN118184332A
CN118184332A CN202410349793.1A CN202410349793A CN118184332A CN 118184332 A CN118184332 A CN 118184332A CN 202410349793 A CN202410349793 A CN 202410349793A CN 118184332 A CN118184332 A CN 118184332A
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calcium
hydroxyapatite
nitrate
bismuth ferrite
composite antibacterial
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庞慧
冯雷
张丰庆
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Jining First People's Hospital Jining Medical Science Research Institute
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Jining First People's Hospital Jining Medical Science Research Institute
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Abstract

The invention discloses a hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biological material and a preparation method thereof. Respectively taking ferric nitrate, bismuth nitrate, calcium nitrate and strontium acetate as solutes and glycol and glacial acetic acid as solvents; calcium nitrate and phosphorus pentoxide are used as solutes and ammonia water is used as a solvent. Mixing and stirring the two matched solutions according to different proportions to obtain a precipitate, and then filtering, cleaning, drying and calcining the precipitate to obtain the composite ceramic powder. The novel hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biological material prepared by the coprecipitation method has good biocompatibility and antibacterial property, and has potential application value in the field of bone tissue engineering.

Description

Hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biological material and preparation method thereof
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biological material and a preparation method thereof.
Background
At present, a plurality of antibacterial materials, such as common inorganic silver ion antibacterial materials, are researched; the main variety of the organic antibacterial agent is vanillin or ethyl vanillin compounds, which are commonly used in polyethylene food packaging films to play an antibacterial role; and photocatalytic antibacterial materials, etc. The antibacterial materials depend on interaction of metal ion charges, hydroxyl radicals and the like with bacteria, so that the active center of protein of the bacteria is destroyed, and microorganisms die or lose division reproductive capacity, thereby achieving the antibacterial effect. However, the material is generally only used for bacteriostasis and antibiosis of the surface of an object, and obviously does not have the characteristics for bacteriostasis of the inside of organisms, particularly for bacteriostasis of some oral cavity materials and orthopedic materials.
For a long time, diseases such as osteoporosis, osteoarthritis, osteomyelitis, bone defects and the like seriously threaten the health of people. The prevalence of the bone diseases in China is relatively high, the research on bone injury type bone diseases is a hot spot in recent years, and researchers are continuously striving to find new and effective treatment methods. Bone implantation is an effective means to solve the above problems, and also promotes the vigorous development of the medical material market, but also brings about a very interesting problem, i.e. how to solve postoperative infection and immune rejection caused by the implant? Infection associated with implants is one of the main causes of failure in orthopedic surgery, where bacteria adhere to the implant surface to form a biofilm, resulting in postoperative infection. However, it is clinically difficult to completely eliminate infection caused by biofilm, and thus, prevention of biofilm formation on implants is one of the most effective strategies for preventing bacterial infection and promoting wound healing. Among various bone materials, hydroxyapatite (Hydroxyapatite, HAP) materials are the closest to natural bone components, have excellent bone conductivity and good biocompatibility, and have been widely studied and applied in the field of bone tissue engineering.
The calcium-strontium doped bismuth ferrite ((CaySr-y) xBi1-xFeO, CSBFO for short) has better ferroelectric and piezoelectric properties, the CSBFO prepared by us has larger self-polarization, that is, CSBFO has obvious coercive field asymmetry and a built-in electric field exists, so CSBFO material has self-spontaneous charges, polarization is not needed when the material with spontaneous polarization is used, and the surface charges have antibacterial action and the action mechanism is to resist adhesion of bacteria on the surface of the material.
The specific mechanism of charge promotion of new bone tissue regeneration, when stimulated by an electrical signal, will activate calcium ion channels, thereby increasing calcium ions in the cell membrane; at the same time, the structure of the membrane receptor is also changed under the action of the local electric field, and the receptor channel is opened, so that calcium ions in the cell membrane can flow in from the endoplasmic reticulum. As the intracellular calcium ion concentration increases, the regulatory proteins and calcineurin are activated, they react with the phosphorylated nuclear factor of the activated cell and then convert it to dephosphorylated activated nuclear factor. These dephosphorylated NF-AT's then translocate to the nucleus and bind to other proteins, resulting in gene transcription. Through gene transcription, the synthesis of transforming growth factors TGF-beta and bone morphogenetic protein BMP-2 is promoted, and the metabolism of cells and the synthesis of extracellular matrixes are finally regulated.
The invention patent CN106478149A discloses a piezoelectric material with antibacterial property and a preparation method and application thereof, the material is more than one of potassium sodium niobate, lithium sodium potassium niobate ceramics or barium titanate, if the antibacterial property of the material is to be exerted, the material is sintered to form the required shape and size, then the ceramics are polarized at 25-125 ℃, the piezoelectric property is only achieved after the polarization, and the piezoelectric property is gradually attenuated along with the extension of the service time. The disadvantage of said patent is that it requires the polarization of the sintered ceramic, the preparation of the electrode during polarization, and the polarization in silicone oil, which is inconvenient for bioceramics and very susceptible to contamination, which is disadvantageous for use.
For this purpose we choose bismuth ferrite doped with calcium and strontium as the base material. In addition, calcium and strontium elements have obvious influence on macrophage polarization, so that the bone immunoregulation effect is good. In view of the above problems, the novel antibacterial composite biological material for the orthopedic implant is prepared, and has excellent self-polarization, good biocompatibility and antibacterial property.
Disclosure of Invention
The invention prepares the composite ceramic material of hydroxyapatite (Ca 5 (PO 4) 3 (OH)) and calcium strontium bismuth ferrite (CaySr-y) xBi1-xFeO3 by a coprecipitation method.
The specific scheme is as follows:
(1) Weighing by an electronic balance according to the molar metering ratio of each solute, wherein the molar ratio of ferric nitrate to bismuth nitrate is 1:1.1, and proper amounts of calcium nitrate and strontium acetate; the ethylene glycol and glacial acetic acid with the volume ratio of 1:3 are measured by a pipette as solvents, PH=5-6 is controlled, the solute and the solution are mixed, and the mixture is placed on a magnetic stirrer for stirring for 12-18 hours until a transparent and clear solution is formed.
(2) Weighing calcium nitrate and phosphorus pentoxide according to a molar metering ratio by using an electronic balance, controlling the molar ratio of calcium to phosphorus to be 5:3, controlling pH to be 8-9 by using ammonia water, and stirring to enable the solution to be a clear solution.
(3) Mixing and stirring the prepared solution according to a proportion to obtain a precipitated precipitate, and then filtering, cleaning and drying the precipitate at 200-300 ℃ by deionized water to obtain precursor powder.
(4) Calcining the precursor powder at 700-800 ℃, and preserving the heat for 1-2 hours to obtain the composite ceramic material.
The invention has the benefits that the novel hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biological material is prepared by a coprecipitation method, the preparation method is simple, and the obtained powder particles are uniform and pure; the composite material has good biocompatibility and antibacterial property, and has potential application value in the field of bone tissue engineering.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Examples
Weighing by an electronic balance according to the molar metering ratio of each solute, wherein the molar ratio of ferric nitrate to bismuth nitrate is 1:1.1, and a proper amount of calcium nitrate; and taking ethylene glycol and glacial acetic acid with a volume ratio of 1:3 as solvents by using a pipette, controlling PH=5, and placing the solute and the solution on a magnetic stirrer for stirring for 12 hours until the solute is completely dissolved. The calcium nitrate and the phosphorus pentoxide are weighed by an electronic balance according to the molar metering ratio, the molar ratio of the calcium to the phosphorus is controlled to be 5:3, the pH=8 is controlled by ammonia water, and the solution is stirred to become a clear solution. Mixing and stirring the solutions according to different ratios to obtain a precipitate, filtering, cleaning and drying the precipitate at 200 ℃ to obtain precursor powder. And calcining the precursor powder at 750 ℃ to obtain the composite ceramic powder.
Examples
Weighing by an electronic balance according to the molar metering ratio of each solute, wherein the molar ratio of ferric nitrate to bismuth nitrate is 1:1.1, and a proper amount of strontium nitrate; and taking ethylene glycol and glacial acetic acid with a volume ratio of 1:3 as solvents by using a pipette, controlling PH=5, and placing the solute and the solution on a magnetic stirrer for stirring for 12 hours until the solute is completely dissolved. The calcium nitrate and the phosphorus pentoxide are weighed by an electronic balance according to the molar metering ratio, the molar ratio of the calcium to the phosphorus is controlled to be 5:3, the pH=8 is controlled by ammonia water, and the solution is stirred to become a clear solution. Mixing and stirring the solutions according to different ratios to obtain a precipitate, filtering, cleaning and drying the precipitate at 200 ℃ to obtain precursor powder. And calcining the precursor powder at 750 ℃ to obtain the composite ceramic powder.
Examples
Weighing by an electronic balance according to the molar metering ratio of each solute, wherein the molar ratio of ferric nitrate to bismuth nitrate is 1:1.1, and the molar ratio of strontium nitrate to calcium nitrate is equal; and taking ethylene glycol and glacial acetic acid with a volume ratio of 1:3 as solvents by using a pipette, controlling PH=5, and placing the solute and the solution on a magnetic stirrer for stirring for 12 hours until the solute is completely dissolved. The calcium nitrate and the phosphorus pentoxide are weighed by an electronic balance according to the molar metering ratio, the molar ratio of the calcium to the phosphorus is controlled to be 5:3, the pH=8 is controlled by ammonia water, and the solution is stirred to become a clear solution. Mixing and stirring the solutions according to different ratios to obtain a precipitate, filtering, cleaning and drying the precipitate at 200 ℃ to obtain precursor powder. And calcining the precursor powder at 750 ℃ to obtain the composite ceramic powder.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.

Claims (6)

1.羟基磷灰石和铁酸钙锶铋复合抑菌生物材料，其特征在于，包括一下原料：硝酸铁、硝酸铋、硝酸钙、乙酸锶、乙二醇、冰乙酸、五氧化二磷、氨水。1. Hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial, characterized in that it includes the following raw materials: ferric nitrate, bismuth nitrate, calcium nitrate, strontium acetate, ethylene glycol, glacial acetic acid, phosphorus pentoxide, and ammonia water. 2.一种如权利要求1所述种羟基磷灰石和铁酸钙锶铋复合抑菌生物材料的制备方法，包括以下步骤：2. A method for preparing the hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial as claimed in claim 1, comprising the following steps: （1）用电子天平按照各溶质的摩尔计量比进行称取，硝酸铁与硝酸铋的摩尔比为1:1.1，以及适量的硝酸钙和乙酸锶；用移液管量取体积比为1:3的乙二醇和冰乙酸作为溶剂，控制PH=5-6，将上述溶质和溶液混合，置于磁力搅拌器上搅拌12-18小时，直至形成透明澄清的溶液；(1) Weighing the solutes according to the molar ratio of each solute using an electronic balance, the molar ratio of ferric nitrate to bismuth nitrate being 1:1.1, and appropriate amounts of calcium nitrate and strontium acetate; using a pipette to measure ethylene glycol and glacial acetic acid in a volume ratio of 1:3 as a solvent, controlling the pH to 5-6, mixing the solutes and the solution, and stirring on a magnetic stirrer for 12-18 hours until a transparent and clear solution is formed; （2）用电子天平按照摩尔计量比进行称取硝酸钙和五氧化二磷，控制钙和磷的摩尔比为5:3, 用氨水来控制pH =8-9, 搅拌使其变为澄清的溶液；(2) Using an electronic balance, weigh calcium nitrate and phosphorus pentoxide according to the molar ratio, control the molar ratio of calcium to phosphorus to be 5:3, use ammonia water to control the pH to 8-9, and stir to make it a clear solution; （3）将上述配置好的上述两种溶液按照比例进行混合搅拌，得到析出沉淀物，然后用去离子水将沉淀物进行过滤、清洗、200-300℃干燥，得到前驱体粉体；(3) Mixing and stirring the two solutions prepared above according to a certain proportion to obtain a precipitate, and then filtering, washing, and drying the precipitate at 200-300° C. with deionized water to obtain a precursor powder; （4）将前驱体粉体在700-800℃煅烧，保温1-2小时，得到复合陶瓷粉体。(4) Calcine the precursor powder at 700-800°C for 1-2 hours to obtain a composite ceramic powder. 3.根据权利要求2 所述羟基磷灰石和铁酸钙锶铋复合抑菌生物材料的制备方法，其特征在于，所述步骤（1）中溶液pH值控制在5-6。3. The method for preparing the hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial according to claim 2, characterized in that the pH value of the solution in step (1) is controlled at 5-6. 4.根据权利要求2 所述羟基磷灰石和铁酸钙锶铋复合抑菌生物材料的制备方法，其特征在于，所述步骤（2）中溶液pH值控制在8-9。4. The method for preparing the hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial according to claim 2, characterized in that the pH value of the solution in step (2) is controlled at 8-9. 5. 根据权利要求2 所述羟基磷灰石和铁酸钙锶铋复合抑菌生物材料的制备方法，其特征在于，所述步骤（3）中沉淀为共沉淀的方法。5. The method for preparing the hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial according to claim 2, characterized in that the precipitation in step (3) is a co-precipitation method. 6.根据权利要求2 所述羟基磷灰石和铁酸钙锶铋复合抑菌生物材料的制备方法，其特征在于，所述步骤（4）中煅烧温度为700-800℃，保温1-2小时。6. The method for preparing the hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial according to claim 2, characterized in that the calcination temperature in step (4) is 700-800°C and the heat preservation time is 1-2 hours.
CN202410349793.1A 2024-03-26 2024-03-26 Hydroxyapatite and calcium strontium bismuth ferrite composite antibacterial biomaterial and preparation method thereof Pending CN118184332A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007091582A (en) * 2005-09-05 2007-04-12 Tokyo Institute Of Technology Oxyapatite containing active oxygen and method for producing the same
CN109432507A (en) * 2018-11-08 2019-03-08 中南大学 The antibacterial hydroxylapatite composite material and preparation method of containing metal oxide
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CN113499485A (en) * 2021-07-08 2021-10-15 深圳先进技术研究院 Lubricating coating for surface of medical instrument and preparation method thereof
CN114534758A (en) * 2022-01-07 2022-05-27 苏州科技大学 Bismuth ferrite/graphite phase carbon nitride composite material and preparation method and application thereof
CN117426603A (en) * 2023-11-24 2024-01-23 济宁市第一人民医院 Shoe pad with antibacterial property and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2007091582A (en) * 2005-09-05 2007-04-12 Tokyo Institute Of Technology Oxyapatite containing active oxygen and method for producing the same
CN109432507A (en) * 2018-11-08 2019-03-08 中南大学 The antibacterial hydroxylapatite composite material and preparation method of containing metal oxide
US20210205085A1 (en) * 2019-11-15 2021-07-08 4Web, Inc. Piezoelectric coated implants and methods of using piezoelectric coated implants to repair bone structures
CN113499485A (en) * 2021-07-08 2021-10-15 深圳先进技术研究院 Lubricating coating for surface of medical instrument and preparation method thereof
CN114534758A (en) * 2022-01-07 2022-05-27 苏州科技大学 Bismuth ferrite/graphite phase carbon nitride composite material and preparation method and application thereof
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