技术领域technical field
本发明涉及钴铬合金，具体地说是用于烤瓷牙冠及冠桥等义齿修复体用钴铬合金。The invention relates to a cobalt-chromium alloy, in particular to a cobalt-chromium alloy used for denture restorations such as porcelain crowns and crown bridges.
背景技术Background technique
牙病患病率在世界各国都很高，就我国而言，牙病患者达8亿之多。而牙体缺损、牙列缺裂和牙列缺失又是牙病中的常见疾病，通常采用义齿进行修复。合金材料强度、硬度、耐磨性、耐久性和韧性等力学性能优良，特别是失蜡铸造技术引入牙科领域后，合金成为主要的修复材料。目前由于镍铬烤瓷合金中镍的潜在致敏和致癌等危害，导致镍铬烤瓷合金逐渐被钴铬烤瓷合金所替代。Dental disease prevalence rate is all very high in countries in the world, and with regard to my country, the dental disease patient reaches as many as 800,000,000. Dental defect, dentition defect and missing dentition are common diseases in dental diseases, and dentures are usually used for restoration. Alloy materials have excellent mechanical properties such as strength, hardness, wear resistance, durability, and toughness. Especially after the lost-wax casting technology is introduced into the dental field, alloys have become the main restoration materials. At present, due to the potential sensitization and carcinogenic hazards of nickel in nickel-chromium ceramic alloys, nickel-chromium ceramic alloys are gradually replaced by cobalt-chromium ceramic alloys.
钴铬烤瓷合金最早应用于移植医疗，用做髋关节之用，由于其耐腐蚀性能较镍基合金好，并且金瓷结合良好，已经成为义齿修复用主要的烤瓷合金。钴基合金是以钴为基体，添加铬、镍、钼和钨等元素形成的合金材料，钴基合金以钴铬钼合金为其典型代表，医用钴基合金具有良好的耐腐蚀性能、耐磨损性能和抗热疲劳性能，热导率高，热膨胀系数较低，杨氏模量不随其强度变化而变化。Cobalt-chromium porcelain alloys were first used in implant medicine for hip joints. Because of their better corrosion resistance than nickel-based alloys and good metal-ceramic bonding, they have become the main porcelain alloys for denture restoration. Cobalt-based alloys are alloy materials formed by adding elements such as chromium, nickel, molybdenum, and tungsten to cobalt. Cobalt-based alloys are typically represented by cobalt-chromium-molybdenum alloys. Medical cobalt-based alloys have good corrosion resistance and wear resistance. Loss performance and thermal fatigue resistance, high thermal conductivity, low thermal expansion coefficient, Young's modulus does not change with its strength.
牙科材料属于生物材料，除了要求合金有高的强度、硬度和延展性，熔点低、流动性好、铸造收缩率小；还要求合金色质优良、合适的热膨胀系数与瓷粉具有良好的匹配；要求有好的流散性以及与包埋材料膨胀系数相适用的收缩系数(即凝固和冷却过程中的收缩)；还要求合金的组织稳定性好，由于长期在口腔中使用，要求合金有很好的生物相容性，抗氧化及耐磨蚀性能。Dental materials are biological materials. In addition to requiring alloys to have high strength, hardness and ductility, low melting point, good fluidity, and low casting shrinkage; they also require alloys with excellent color quality, suitable thermal expansion coefficients and porcelain powders to have a good match; It is required to have good fluidity and a shrinkage coefficient suitable for the expansion coefficient of the embedding material (that is, shrinkage during solidification and cooling); it also requires good structural stability of the alloy. Due to long-term use in the oral cavity, the alloy is required to have a good Excellent biocompatibility, oxidation resistance and abrasion resistance.
发明内容Contents of the invention
本发明的目的在于提供一种钴基烤瓷合金，考虑到钴是一种重要战略资源，世界上大多数国家缺钴，钴的价格昂贵等问题，本发明在钴铬钼合金基础上，降低钴和铬的含量，适量加入铁元素和锰元素，并加入氮元素来优化力学性能和耐蚀性能。同时考虑到口腔环境细菌数量和种类繁杂，加入适量铜元素。本发明钴基烤瓷合金具有优良的抗菌功能和金瓷结合能力，同时具有优良的力学性能和耐蚀性能，不含潜在致敏等危害的镍元素，且低成本，对义齿修复具有重要意义，具有重要的社会和经济意义。The object of the present invention is to provide a kind of cobalt-based ceramic alloy, considering that cobalt is a kind of important strategic resource, most countries in the world lack cobalt, the price of cobalt is expensive etc., the present invention is based on cobalt chromium molybdenum alloy, reduces The content of cobalt and chromium, appropriate amount of iron and manganese, and nitrogen are added to optimize the mechanical properties and corrosion resistance. At the same time, considering the number and types of bacteria in the oral environment, an appropriate amount of copper is added. The cobalt-based ceramic alloy of the present invention has excellent antibacterial function and metal-ceramic bonding ability, and at the same time has excellent mechanical properties and corrosion resistance, does not contain potentially harmful nickel elements such as sensitization, and is low in cost, which is of great significance for denture restoration , has important social and economic significance.
基于以上目的，本发明提供了一种钴基烤瓷合金，其特征在于：按重量计其化学成分为：碳C≤0.08％，铬Cr：16～24％，铁Fe：10～20％，锰Mn：5～15％，钼Mo：2～8％，钨W：2～8％，铜Cu：1～3％，氮N≤0.4％，镍Ni≤0.1％，硫S＜0.01％，磷P＜0.02％，钴Co：余量。优选为：碳C≤0.08％，铬Cr：20～24％，铁Fe：16-18％，锰Mn：8-12％，钼Mo：4～6％，钨W：2～4％，铜Cu：1～3％，氮N：0.2～0.4％，镍Ni≤0.1％，硫S＜0.01％，磷P＜0.02％，钴Co：余量。Based on the above purpose, the present invention provides a cobalt-based ceramic alloy, characterized in that: by weight, its chemical composition is: carbon C≤0.08%, chromium Cr: 16-24%, iron Fe: 10-20%, Manganese Mn: 5-15%, Molybdenum Mo: 2-8%, Tungsten W: 2-8%, Copper Cu: 1-3%, Nitrogen N≤0.4%, Nickel Ni≤0.1%, Sulfur S<0.01%, Phosphorus P<0.02%, cobalt Co: balance. Preferably: carbon C≤0.08%, chromium Cr: 20-24%, iron Fe: 16-18%, manganese Mn: 8-12%, molybdenum Mo: 4-6%, tungsten W: 2-4%, copper Cu: 1-3%, nitrogen N: 0.2-0.4%, nickel Ni≤0.1%, sulfur S<0.01%, phosphorus P<0.02%, cobalt Co: balance.
本发明所提供的钴基烤瓷合金中，为了避免镍元素的潜在致敏和致癌等危害，考虑到冶金原料中镍的残余含量，本发明钴基合金中控制镍Ni≤0.1(wt％)。In the cobalt-based ceramic alloy provided by the present invention, in order to avoid the potential sensitization and carcinogenic hazards of nickel elements, considering the residual content of nickel in metallurgical raw materials, the nickel Ni in the cobalt-based alloy of the present invention is controlled to be less than or equal to 0.1 (wt%).
本发明所提供的钴基烤瓷合金，为了保证优良的力学性能和耐蚀性能，避免合金中过多的碳化物形成，本发明钴基烤瓷合金中碳含量最好控制在C≤0.08(wt％)For the cobalt-based ceramic alloy provided by the present invention, in order to ensure excellent mechanical properties and corrosion resistance, and avoid excessive carbide formation in the alloy, the carbon content in the cobalt-based ceramic alloy of the present invention is preferably controlled at C≤0.08( wt%)
本发明所提供的钴基烤瓷合金含有氮元素，首先氮有助于提高合金的强度和耐腐蚀性，根据点蚀和缝隙腐蚀抗力近似计算公式PREN＝％Cr+3.3％Mo+(13-30)％N，可以看出氮和铬、钼共同作用是铬单独作用效果的20～30倍。其次合金中的氮元素在人体内是宏量元素，对人体没有危害。因此考虑到冶金学因素的影响，本发明钴基烤瓷合金中氮含量控制在N≤0.4％。The cobalt-based ceramic alloy provided by the present invention contains nitrogen element, at first nitrogen helps to improve the strength and corrosion resistance of the alloy, according to the approximate calculation formula of pitting and crevice corrosion resistance PREN=%Cr+3.3%Mo+(13-30 )% N, it can be seen that the combined effect of nitrogen, chromium and molybdenum is 20 to 30 times that of chromium alone. Secondly, the nitrogen element in the alloy is a macro element in the human body and has no harm to the human body. Therefore, taking into account the influence of metallurgical factors, the nitrogen content in the cobalt-based ceramic alloy of the present invention is controlled at N≤0.4%.
本发明所提供的钴基烤瓷合金含有铬元素，铬是提高钴基合金耐蚀性最主要的合金元素，在氧化介质中，铬能使合金表面上迅速生成氧化铬(例如Cr2O3)的钝化膜，这层钝化膜是非常致密和稳定的，即使一旦被破坏也能迅速恢复。铬同时非常有效地提高钴基合金的耐点蚀性能，当合金中有钼和氮同时存在时，铬的这种有效性大大加强。由于铬是不锈钢中主要的耐蚀元素，而且也提高合金中氮的溶解度，因此本发明钴基烤瓷合金中铬含量控制在16～24％。The cobalt-based ceramic alloy provided by the present invention contains chromium element, and chromium is the most important alloying element to improve the corrosion resistance of the cobalt-based alloy. In an oxidizing medium, chromium can rapidly generate chromium oxide (such as Cr2 O3 ) passivation film, this layer of passivation film is very dense and stable, even if it is damaged, it can recover quickly. Chromium is also very effective in improving the pitting corrosion resistance of cobalt-based alloys. This effectiveness of chromium is greatly enhanced when molybdenum and nitrogen are present in the alloy. Since chromium is the main anti-corrosion element in stainless steel and also improves the solubility of nitrogen in the alloy, the content of chromium in the cobalt-based ceramic alloy of the present invention is controlled at 16-24%.
本发明所提供的钴基烤瓷合金含有铁元素，首先铁是一种人体必需的微量元素，参与人体大多数新陈代谢。其次本发明钴基烤瓷合金中铁元素的加入主要是用来替代合金中部分昂贵的钴元素，以达到降低成本的目的。在合金中铁可以和钴形成连续的固溶体，不影响钴基合金的性能，本发明钴基烤瓷合金中铁含量控制在10～20％。The cobalt-based ceramic alloy provided by the present invention contains iron element. Firstly, iron is an essential trace element for the human body and participates in most of the metabolism of the human body. Secondly, the addition of the iron element in the cobalt-based ceramic alloy of the present invention is mainly used to replace part of the expensive cobalt element in the alloy, so as to achieve the purpose of reducing costs. In the alloy, iron can form a continuous solid solution with cobalt, which does not affect the performance of the cobalt-based alloy. The content of iron in the cobalt-based ceramic alloy of the invention is controlled at 10-20%.
本发明所提供的钴基烤瓷合金含有钼元素，首先钼是一种重要的人体必需微量元素。其次钼加入钴基合金中主要用来提高合金的耐蚀性特别是耐点蚀及缝隙腐蚀等性能。研究文献表明钼的耐点蚀及缝隙腐蚀的能力为铬的3倍左右，大量实验指出，钼主要是强化钢中铬的耐蚀作用。因此本发明钴基烤瓷合金中钼含量控制在2～8％。The cobalt-based ceramic alloy provided by the present invention contains molybdenum element, firstly, molybdenum is an important essential trace element for human body. Secondly, adding molybdenum to cobalt-based alloys is mainly used to improve the corrosion resistance of the alloy, especially the resistance to pitting corrosion and crevice corrosion. Research literature shows that the ability of molybdenum to resist pitting corrosion and crevice corrosion is about 3 times that of chromium. A large number of experiments have pointed out that molybdenum mainly strengthens the corrosion resistance of chromium in steel. Therefore, the content of molybdenum in the cobalt-based ceramic alloy of the present invention is controlled at 2-8%.
本发明所提供的钴基烤瓷合金含有锰元素，首先锰是人体必需的微量元素，锰在动植物及人体内均有重要的作用，是酶的辅因子，可促进维生素合成，锰参与蛋白质的合成代谢，还能激活DNA聚合酶等。其次合金中的锰元素是奥氏体形成元素，具有强烈稳定钴基合金奥氏体基体的作用。在本发明合金中锰元素最重要的作用是增加合金中氮的溶解度，调整合金中氮的含量，考虑到合金中的氮含量，因此本发明钴基烤瓷合金中锰含量控制在5～15％。The cobalt-based ceramic alloy provided by the present invention contains manganese element. First, manganese is an essential trace element for the human body. Manganese plays an important role in animals, plants and the human body. It is a cofactor of enzymes and can promote vitamin synthesis. Manganese participates in protein It can also activate DNA polymerase and so on. Secondly, the manganese element in the alloy is an austenite forming element, which has a strong role in stabilizing the austenite matrix of the cobalt-based alloy. The most important effect of the manganese element in the alloy of the present invention is to increase the solubility of nitrogen in the alloy and adjust the content of nitrogen in the alloy. Considering the nitrogen content in the alloy, the content of manganese in the cobalt-based ceramic alloy of the present invention is controlled at 5-15 %.
本发明所提供的钴基烤瓷合金含有钨元素，钨的加入主要是为了调整由于铁和锰元素加入造成的合金密度，弹性模量和热膨胀系数等物理量的变化，由于热膨胀系数和材料的密度关系密切，因此通过加入不同含量的钨来调整本发明钴基烤瓷合金的热膨胀系数，使其具有优良的金瓷结合力。因此本发明钴基烤瓷合金中钨含量控制在2～8％。The cobalt-based ceramic alloy provided by the present invention contains tungsten element, and the addition of tungsten is mainly to adjust the alloy density caused by the addition of iron and manganese elements, changes in physical quantities such as elastic modulus and thermal expansion coefficient, due to the thermal expansion coefficient and the density of the material Therefore, the thermal expansion coefficient of the cobalt-based ceramic alloy of the present invention is adjusted by adding different contents of tungsten, so that it has excellent metal-ceramic bonding force. Therefore, the tungsten content in the cobalt-based porcelain alloy of the present invention is controlled at 2-8%.
本发明所提供的钴基烤瓷合金含有铜元素，铜的加入一方面可以降低合金的熔点，增强流动性。另一方面铜是本发明钴基烤瓷合金具有抗菌功能的必要条件，铜元素在钴中的溶解度随着温度降低逐渐下降，因此本发明烤瓷合金可以通过特殊抗菌热处理(热处理工艺为：400-500℃保温0.5-5h)，使部分富铜相能在合金基体中均匀弥散析出，从而赋予钴铬烤瓷合金广谱抗菌功能。考虑到过多的铜含量影响合金的热加工性能，因此本发明钴基烤瓷合金中铜含量控制在1～3％。The cobalt-based ceramic alloy provided by the invention contains copper element, and the addition of copper can lower the melting point of the alloy and enhance fluidity. On the other hand, copper is a necessary condition for the cobalt-based ceramic alloy of the present invention to have antibacterial function, and the solubility of copper element in cobalt gradually decreases as the temperature decreases, so the ceramic alloy of the present invention can be passed through special antibacterial heat treatment (heat treatment process is: 400 -500°C for 0.5-5h), so that part of the copper-rich phase can be uniformly dispersed and precipitated in the alloy matrix, thereby endowing the cobalt-chromium ceramic alloy with a broad-spectrum antibacterial function. Considering that excessive copper content affects the hot workability of the alloy, the copper content in the cobalt-based ceramic alloy of the present invention is controlled at 1-3%.
在本发明所提供的钴基烤瓷合金中，硫和磷被视为有害杂质，由于本发明钴基烤瓷合金中需要通过调整锰含量来调整氮含量，为了避免硫化锰杂质的形成，本发明钴基合金中控制硫含量应低于0.01％，控制磷含量在0.02％以下。In the cobalt-based ceramic alloy provided by the present invention, sulfur and phosphorus are regarded as harmful impurities, because the nitrogen content needs to be adjusted by adjusting the manganese content in the cobalt-based ceramic alloy of the present invention, in order to avoid the formation of manganese sulfide impurities, this The sulfur content in the invented cobalt-based alloy should be controlled below 0.01%, and the phosphorus content should be controlled below 0.02%.
本发明还提供了上述钴铬烤瓷合金的抗菌热处理工艺，具体工艺为：在1150℃-1200℃保温0.5-2h，使合金中的铜能充分均匀地固溶于基体中，水冷至室温后，根据合金中的铜含量高低，在400℃-500℃保温0.5-5h，使部分铜从合金中析出足够量的富铜相，保证一定的抗菌能力。The present invention also provides an antibacterial heat treatment process for the above-mentioned cobalt-chromium ceramic alloy. The specific process is: heat preservation at 1150°C-1200°C for 0.5-2h, so that the copper in the alloy can be fully and uniformly dissolved in the matrix, and then water-cooled to room temperature , according to the copper content in the alloy, keep it at 400°C-500°C for 0.5-5h, so that part of the copper will precipitate a sufficient amount of copper-rich phase from the alloy to ensure a certain antibacterial ability.
本发明所提供的钴基烤瓷合金的优势：The advantages of the cobalt-based ceramic alloy provided by the present invention:
首先对比临床应用的钴铬钼烤瓷合金，合金中添加了铜元素，通过特殊热处理后，使合金具有一定的抗菌性能，在口腔环境中使用有助于缓解牙龈发炎等口腔疾病。First of all, compared with the cobalt-chromium-molybdenum porcelain alloy in clinical application, copper element is added to the alloy. After special heat treatment, the alloy has certain antibacterial properties, which can help relieve oral diseases such as gingival inflammation when used in the oral environment.
其次通过加入铁、锰和氮元素代替部分昂贵钴元素，有效地降低了钴基合金的制备成本。铁和锰元素都是人体必需的微量元素，对人体没有严重危害。合金中添加的氮元素是有效的奥氏体稳定元素，同时可有有效提高合金的力学性能和耐蚀性能。Secondly, by adding iron, manganese and nitrogen elements to replace some expensive cobalt elements, the preparation cost of cobalt-based alloys is effectively reduced. Both iron and manganese are essential trace elements for the human body and have no serious harm to the human body. The nitrogen element added to the alloy is an effective austenite stabilizing element, and can effectively improve the mechanical properties and corrosion resistance of the alloy.
第三，烤瓷合金的热膨胀系数通过其中的钨元素含量来调整，根据不同的瓷粉，可以调整合金成分，获得与瓷粉热膨胀系数完美配合的烤瓷合金，最终具有优良的金瓷结合力。Third, the thermal expansion coefficient of the porcelain alloy is adjusted by the tungsten element content in it. According to different porcelain powders, the alloy composition can be adjusted to obtain a porcelain alloy that perfectly matches the thermal expansion coefficient of the porcelain powder, and finally has excellent metal-ceramic bonding force .
第四，烤瓷合金具有优良的塑韧性，有希望改变传统的铸造成型方法为压力成型。Fourth, porcelain alloys have excellent plasticity and toughness, and it is hopeful to change the traditional casting molding method to pressure molding.
应用范围：Applications:
本发明钴基烤瓷合金，相对于传统的钴基合金，具有一定的抗菌功能以及优良的力学和耐蚀性能，并且成本低，作为烤瓷合金具有极大的优势，可作为牙科材料广泛用于义齿修复材料及修复体，如制作各种牙用嵌体、3/4冠、全冠、镶面冠、短跨度桥和长跨度桥等，也可应用于骨科等外科植入领域和食品餐饮器械、钟表、首饰等领域。Compared with traditional cobalt-based alloys, the cobalt-based ceramic alloy of the present invention has certain antibacterial function, excellent mechanical and corrosion resistance properties, and low cost, and has great advantages as a ceramic alloy, and can be widely used as dental materials Used in denture restoration materials and restorations, such as making various dental inlays, 3/4 crowns, full crowns, veneered crowns, short-span bridges and long-span bridges, etc. It can also be used in orthopedics and other surgical implant fields and food Catering equipment, watches, jewelry and other fields.
具体实施方式Detailed ways
本发明牙科用钴铬合金采用普通真空感应炉冶炼，浇铸成合适尺寸的棒材，所得牙科钴铬合金铸态棒材的相关物理性能及力学性能：熔点＝1400-1550，热膨胀系数＝13.8-14.9×10-6，σb≥880MPa，σ0.2≥500MPa，δ5≥8％，Ψ≥5％，Hv5≥260，合金与瓷之间的结合力可高达300Mpa以上。The dental cobalt-chromium alloy of the present invention is smelted in an ordinary vacuum induction furnace and cast into bars of suitable size. The relevant physical properties and mechanical properties of the as-cast dental cobalt-chromium alloy bars obtained are: melting point=1400-1550, thermal expansion coefficient=13.8- 14.9×10-6, σb≥880MPa, σ0.2≥500MPa, δ5≥8%, Ψ≥5%, Hv5≥260, the bonding force between alloy and porcelain can be as high as 300Mpa or more.
实施例：Example:
根据本发明所设定的化学成分范围，在25公斤容量真空感应炉内冶炼了4炉钢及1炉对比合金各10公斤，其具体化学成分如表1所示。本发明合金钢锭在1150℃-1200℃保温2h，锻造成30mm厚板材，然后在1150℃保温2h使合金中的铜能充分均匀地固溶于基体中，水冷至室温后，使钢中的铜处于过饱和状态。合金1在400℃保温5h，合金2和3分别在500℃保温3h和2h，优选成分合金4在450℃保温3h，测得的力学性能如表2所示。According to the chemical composition range set by the present invention, 4 furnaces of steel and 10 kg of contrast alloy were smelted in a vacuum induction furnace with a capacity of 25 kg. The specific chemical compositions are as shown in Table 1. The alloy steel ingot of the present invention is kept at 1150°C-1200°C for 2h, forged into a 30mm thick plate, and then kept at 1150°C for 2h so that the copper in the alloy can be fully and uniformly dissolved in the matrix, and after water cooling to room temperature, the copper in the steel in a state of supersaturation. Alloy 1 was held at 400°C for 5 hours, alloys 2 and 3 were held at 500°C for 3 hours and 2 hours respectively, and the preferred component alloy 4 was held at 450°C for 3 hours. The measured mechanical properties are shown in Table 2.
由实施例测试结果可知，本发明钴基烤瓷合金通过加入铁和锰合金代替昂贵的钴合金，并通过提高氮含量降低碳含量，相比临床使用的烤瓷用钴铬钼合金(对比合金)，不但保证较高的强度，同时成倍提高了合金的塑韧性，表现出明显的性价比。优选合金4强度性能最接近对比用烤瓷合金，但是塑韧性更好，有利于合金的成型，改变传统的铸造成型为塑性变形压力成型。As can be seen from the test results of the examples, the cobalt-based ceramic alloy of the present invention replaces expensive cobalt alloys by adding iron and manganese alloys, and reduces the carbon content by increasing the nitrogen content. ), not only ensures higher strength, but also doubles the plasticity and toughness of the alloy, showing obvious cost performance. The preferred alloy 4 has the closest strength and performance to the comparative ceramic alloy, but has better plasticity and toughness, which is beneficial to the forming of the alloy, and the traditional casting forming is changed to plastic deformation pressure forming.
表1本发明钴铬合金的化学成分The chemical composition of table 1 cobalt-chromium alloy of the present invention
表2本发明钴铬合金的力学性能The mechanical property of table 2 cobalt-chromium alloy of the present invention
上述实施例只为说明本发明的技术构思及特点，其目的在于让熟悉此项技术的人士能够了解本发明的内容并据以实施，并不能以此限制本发明的保护范围。凡根据本发明精神实质所作的等效变化或修饰，都应涵盖在本发明的保护范围之内。The above-mentioned embodiments are only to illustrate the technical concept and characteristics of the present invention, and the purpose is to enable those skilled in the art to understand the content of the present invention and implement it accordingly, and not to limit the protection scope of the present invention. All equivalent changes or modifications made according to the spirit of the present invention shall fall within the protection scope of the present invention.
| Application Number | Priority Date | Filing Date | Title |
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| CN201310151449.3ACN103233143B (en) | 2013-04-26 | 2013-04-26 | A kind of cobalt-based porcelain alloy and application thereof |
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| CN201310151449.3ACN103233143B (en) | 2013-04-26 | 2013-04-26 | A kind of cobalt-based porcelain alloy and application thereof |
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