CN1475317A - Oral carity cast titanium special embedded material and its preparation method and use - Google Patents
Oral carity cast titanium special embedded material and its preparation method and use Download PDFInfo
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- CN1475317A CN1475317A CNA031353347A CN03135334A CN1475317A CN 1475317 A CN1475317 A CN 1475317A CN A031353347 A CNA031353347 A CN A031353347A CN 03135334 A CN03135334 A CN 03135334A CN 1475317 A CN1475317 A CN 1475317A
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Abstract
An embedding material for casting the titanium part used in oral cavity is prepared from Al2O3, MgO, Mg(H2PO4)2.2HO2, NH4H2PO4, metal Zr powder and AlF3 through proportionally mixing them with liquid, embedding mould, solidifying, heating to 120-160 deg.C, holding, the temp for 60-100 min, heating to 700-850 deg.C, holding the temp for 80-100 min, heating to 1100-1250 deg.C, holding the temp for 1-3 hr, slow cooling to 600-800 deg.C, casting titanium, and cooling in cold water.
Description
One, the technical field
The invention relates to an embedding material special for oral cavity titanium casting, a preparation method and application thereof, and belongs to the field of precise casting embedding materials for oral cavity clinical restoration.
Second, background Art
Pure Titanium and Titanium alloys have the characteristics of light specific gravity, high strength, low elastic modulus, good corrosion resistance and the like, and in the 50 th century of the 20 th century, Eugene P.Lantenschlager and other 'Titanium and Titanium alloys' International Dental Journal 1993; 43: 245-253, pure titanium and titanium alloys have been reported to be used as important aviation materials in the aviation field, and Pusu cloud, et al, published by "metal implant materials and corrosion thereof," Beijing aerospace and aviation university, it is believed that pure titanium and titanium alloys are biological metals due to their good biocompatibility, and have been used in dental clinic for a long time. The oral tissue has high requirements on the aspects of shape, strength, precision and the like of a repaired body due to the special structure and function of the oral tissue, and the oral tissue is prepared from Zhao Yun Feng (oral repair technology and technology), Sichuan university Press, 2001: precision casting is believed to be the primary method of forming dental restorations 29. Because pure titanium has small specific gravity, high melting point and extremely active chemical properties at high temperature, and can chemically react with nitrogen, hydrogen, oxygen in the air, casting embedding materials, crucibles and the like to cause pollution and modification on the surface of a casting, the casting of titanium can be finished by special equipment and technology, and the requirement on a casting system is strict, so the method cannot be popularized and applied. With the improvement of the industrial level in the early eighties, the continuous improvement of a titanium casting machine and the development of casting embedding materials, and the research of titanium casting in the oral cavity field is carried out successively in industrially developed countries. Berg E et al, in the article "Dentists' opinions of cast titanium restorings" [ J Dent]1997, 25: 113-117 is considered to gradually mature at present after decades of efforts, and shows good application prospects. Zhang in thesis "influence of roasting and casting temperature on surface structure of pure titanium casting" [ journal of oral material instruments]1993, 2 (4): 3-7; takahashi J, Zhang JZ et al, "Castability and hardness of cast plates from experimental-bonded silicon inventers molds" [ Dent Mater J]1993, 12 (2): 238-241; MiyakawaO, Watanabe K et al, "layred structure of cast titanium surface" [ Dent Mater]1989, 8 (2): 175, the development of a dental titanium casting machine is considered to be more and more complete today, and the development of a new embedding material becomes a key for protecting the original biological and physical properties of pure titanium and improving the casting precision and quality.
The melting point of titanium is 1668 ℃, and a cast titanium embedding material is called an ultra-high temperature embedding material, and is mainly composed of a refractory material and a binder, in order to obtain a cast denture with good dimensional accuracy, it is necessary to compensate for the casting shrinkage of metal by the hardening expansion and thermal expansion of the embedding material, the casting shrinkage of pure titanium is 1.8 to 2.0%, and therefore, itis necessary to compensate for the metal shrinkage in this range in the casting of pure titanium, the cast titanium embedding material must have basic conditions that ① reacts slightly with molten titanium to obtain good surface properties, ② does not contaminate the casting, ③ has a moderate expansion to compensate for the casting shrinkage, and these have been confirmed in studies by the researchers in the field, チタンわよタン alloy mechanics 1992, 20 (12): 1264, engineering, and "dental titanium casting system": 1997, 14 (4): 388-39, valley チタン, "macro- つを", and させゐ (1993), 8521, 1993).
As for the research of the embedding material special for casting titanium, Miyakawa, a scholars of Japan, first conducted the research of casting titanium by using common high temperature phosphate and quartz embedding material, and then, with the progress of the titanium casting technology, the research of the embedding material of casting titanium in various countries has been progressed, and various products such as RematitanPlus embedding material of DENTAURUM, Germany, Titavet ME-MZ embedding material of Japan, CD titan investing embedding material of Japan Songfeng have been developed, but there are still defects in the expansion amount of the embedding material, the reaction with molten titanium, and the like. The refractory material of the silicon-based titanium casting embedding material is cristobalite and quartz, the embedding material has sufficient expansion rate and good operability, but is reactive with molten titanium to cause embrittlement, modification and pollution on the surface of a casting; the magnesium system has the outstanding advantages of smooth casting surface and little pollution, and has the main defects of insufficient expansion amount and lower mold strength; the aluminum system embedded material has stable volume at high temperature, compact structure and difficult cracking, and has the defects of long hardening and mold roasting time, hard mold and poor mold release property; the casting obtained by the zirconium embedding material has smooth surface and good demoulding performance, but the expansion amount is not stable, the price is expensive, and in addition, the operation performance is still to be improved.
In a word, the embedding material used for titanium casting at present has the problems of great reaction of ① and molten titanium, insufficient expansion amount of ②, long hardening time of ③, poor operability, crack generation of shrinkage deformation during ④ sintering, high price of ⑤ and the like, which are difficult to solve, the high-quality titanium casting embedding material is not published at present, and the development of a new embedding material for improving the quality of titanium castings is a target which is continuously pursued by broad students.
Third, the invention
The invention aims to provide a special embedding material for oral titanium casting and a preparation method and application thereof aiming at the defects of the prior art, and is characterized in that the characteristic that magnesia and alumina generate magnesia-alumina spinel in a solid-phase reaction to generate volume expansion is utilized, the magnesia and the alumina are used as refractory materials according to a certain proportion, and the thermal expansion rate of the embedding material is controlled by adjusting the granularity of powder, so that the purpose of generating enough volume expansion at lower temperature to compensate for the casting shrinkage of pure titanium is achieved.
The inventor finds that the refractory filler is a main body material in the tissue structure of the unshaped refractory material, plays a role of a framework, determines the physical mechanics and high-temperature use performance of the refractory filler, and the self-developed refractory filler of the oral cast titanium embedding material is MgO and Al2O3And MgAl formed at high temperature2O4. As a raw material for sintering spinel, Al is most suitable2O3The source is sintered alumina, followed by tabular alumina, highly active light alumina and nearly chemically inert fused corundum are not suitable, while the best source of MgO is sintered magnesia, hence Al in the oral embedding material2O3Sintered alumina is adopted, and MgO is sintered into heavy magnesia by adopting light magnesia and then is subjected to ball milling treatment.
From the chemical thermodynamic analysis, the common refractory oxides can be arranged according to the chemical stability of the refractory oxides to the titanium liquid:
SiO2＜Al2O3＜MgO＜CaO＜ZrO2＜Y2O3＜ThO2wherein SiO is2Has a free energy of formation (G) higher than that of TiO2Titanium and SiO at 1000 deg.C2The contact can generate reduction reaction: reduced Si is TiO2Dissolving and eutectic to produce titanium oxide and titanium silicide. The free energy of other refractory oxides is all higher than that of TiO2Low, i.e. more reducing, so that none of these oxides theoretically would undergo a reduction reaction with molten titanium, and therefore these oxides (Al) were selected for use in self-developed oral cast titanium embedding materials2O3MgO) as the titanium casting embedding material can reduce the reaction with molten titanium and improve the quality of titanium castings.
The binder is a material which can enable the refractory filler and the additive to be cemented together and show certain strength. The binding agent is an important component of unshaped refractory material, and the binding agent of embedding material in dental precision casting is generally made of phosphate, such as NH4H2PO4And Mg (H)2PO4)2·2H2And O, wherein the embedding material of the phosphate system has good fluidity, proper hardening time and high compressive strength, and the embedding material except the phosphate system has longer hardening time, is lack of hardening expansion and has low compressive strength of the casting mold. The special embedding material for oral titanium casting adopts NH4H2PO4And Mg (H)2PO4)2·2H2O as a binder, can suitably reduce NH4H2PO4The amount of the catalyst is reduced, thereby reducing the generation of ammonia gas in the baking process of the casting mould and reducing the influence of reaction products on the casting.
In addition to the binder and refractory filler, additives can be added to the embedding material to strengthen the binder and improve the performanceThe overall properties of the investment. Special embedding for oral titanium castingA small amount of metal zirconium powder is added into the material, and the volume expansion caused by the reaction of the metal zirconium powder with oxygen and nitrogen at high temperature to generate zirconium oxide, nitride and zirconium oxynitride is utilized to increase the thermal expansion amount of the embedding material so as to compensate the metal shrinkage in casting. AlF3The addition of the catalyst reduces the temperature of the generated magnesium aluminate spinel by over 200 ℃, and a large amount of magnesium aluminate spinel is generated at 900 ℃. Because the synthesis reaction of the magnesium aluminate spinel can bring expansion of volume, a small amount of AlF is added into the embedding material special for oral titanium casting3The aim is to reduce the generation temperature of the magnesium aluminate spinel, so that the embedding material has enough thermal expansion at the baking temperature of the casting mould, and the precision of the casting is improved. Due to AlF3Sublimating at about 1200 ℃, so that the baked embedding material does not contain AlF3And the performance of the titanium casting cannot be adversely affected.
The aim of the invention is realized by the following technical measures, wherein the parts of the raw materials are parts by weight except for special specifications.
1. The special embedding material for oral cavity cast titanium comprises the following components in parts by weight:
Al2O320～70
MgO 15～60
Mg(H2PO4)2·2HO23～15
NH4H2PO41～10
Zr 1～10
AlF31～10
the powder and the mixing liquid are 100: 20-40
Wherein the mixing solution is at least one of water, silica sol and/or ethyl acetate.
2. The preparation method of the special embedding material for oral cavity titanium casting comprises the following steps:
al with a particle size of 0.8 to 180 μm2O320 to 70 parts of MgO with a particle size of 5 to 15 μm and Mg (H) with a particle size of 50 to 90 μm2PO4)2·2HO23 to 15 parts and NH4H2PO41-10 parts of metal zirconium powder and 1-10 parts of AlF31-10 parts of the raw materials are added into a ball mill to be ground and mixed uniformly for later use.
3. The application of the special embedding material for oral cavity cast titanium comprises the following steps:
uniformly mixing the embedding material according to the proportion of powder to mixing liquid of 100: 20-40, embedding a casting mold, taking down a casting ring after the embedding material is solidified and hardened, and sintering the casting mold in an automatic oven special for titanium casting, wherein the baking procedure of the casting mold is as follows: raising the temperature from room temperature to 120-160 ℃ for 60-100 min, raising the temperature to 700-850 ℃ for 80-100 min, continuing raising the temperature to 1100-1250 ℃ for 1-3 h, then slowly lowering the temperature to 600-800 ℃, wherein the raising and lowering speed is about 5 ℃/min, after 10-12 h, putting the casting mold with the constant temperature of 600-800 ℃ into a titanium casting machine for casting without a ring, quenching the cast casting mold in cold water, removing the embedding material on the surface of the casting, and performing sand blasting treatment to obtain the required casting.
The invention has the following advantages:
experimental test results of material performance show that the main physical and chemical properties of the oral cavity cast titanium embedding material basically meet the requirements of clinical oral cavity repair precision casting; the performance indexes of the casting in all aspects such as casting flow rate, surface roughness, surface hardening layer thickness, element invasion pollution and the like can meet the clinical application, and the performance is excellent; the research result of the casting precision further proves that the oral cavity casttitanium embedding material has good casting precision and is suitable for clinical application.
The method comprises the following steps of measuring various physical and chemical performance indexes of the special embedding material for oral cavity cast titanium and comparing the difference of the special embedding material for oral cavity cast titanium and the special embedded material for Rematitan Plus clinically used cast titanium to the casting precision of pure titanium, wherein the results are as follows:
1. the solidification time of the oral cavity titanium casting embedding material is 10.236 +/-0.31801 min; the powder-liquid ratio is reduced, the solidification time is prolonged (P is less than 0.01); the heat generation temperature of the solidification reaction is 57.2 +/-0.83 ℃; the flowability was 62.6. + -. 1.22mm (initial diameter 28 mm).
2. The normal temperature compressive strength is 7.86 +/-0.710 MPa (after being dried for 24 hours); the normal temperature compressive strength is increased (P is less than 0.01) along with the time; after quenching at the high temperature of 1100 ℃, the residual compressive strength is 2.46 +/-0.791 MPa.
3. 2hr after stirring, the maximum solidification expansion is 1.27%, and the final solidification expansion is 1.26%; the maximum thermal expansion rate of the casting mold is 0.8235% when the casting mold is heated to 1000 ℃, and the thermal expansion rate of the casting mold is 0.6124% when the casting temperature is reduced to 800 ℃. At the casting temperature of 800 ℃, the total expansion rate of the oral cavity cast titanium embedding material is 1.8724%, the casting shrinkage rate is close to 1.8-2.0% of pure titanium, and the volume shrinkage of a titanium casting can be compensated.
4. The practical refractoriness is higher than 1700 ℃, and the casting requirement of pure titanium in oral clinic is completely met.
5. The casting is carried out at the temperature of 600 ℃ and 800 ℃ of the casting mould, and the casting flow rate of the pure titanium grid casting reaches 100 percent.
6. The surface roughness Ra of the pure titanium casting of the oral cavity titanium casting embedding material is 1.7211 +/-0.08054 mu m, and is smaller than the surface roughness Ra of 1.9067 +/-0.15116 mu m of the pure titanium casting of the embedding material special for the Rematian Plus titanium casting, and the difference has statistical significance (P is less than 0.05).
7. The surface hardening layer of the pure titanium casting of the oral cavity casting titanium embedding material is 50 microns and is smaller than the surface hardening layer (140 microns) of the pure titanium casting of the Rematitan Plus special casting titanium embedding material.
8. The porosity of the cast product cast by the oral cavity cast titanium embedding material is 0.044%, and the average diameter of the air holes is 0.10 mm. Does not affect the mechanical property of the cast titanium and meets the requirement of oral clinical application.
9. Scanning electron microscope and metallographic microscopic observation of the cast product cast by the oral cavity cast titanium embedding material show that the interface between the surface layer of the pure titanium cast product cast by the oral cavity cast titanium embedding material and the casting mould is flat, no sintered layer and α layers are seen, no silicon-rich layer in the titanium cast product is observed, the needle-shaped crystal layer is thin, and the boundary with the titanium matrix is not clear.
10. The element energy spectrum analysis shows that the surface pollution of the pure titanium casting is small, the reaction layer is thin, and the penetration depth of the embedded material constituent elements in the reaction layer is shallow.
11. The suitability of the pure titanium full crown cast by the oral cavity cast titanium embedding material is less than 45 mu m, and the suitability of the pure titanium cast bracket is 89.5 +/-1.59 mu m, which is in a clinically acceptable range.
Fourth, detailed description of the invention
The present invention is described in detail below by way of examples, it should be noted that the examples are only for illustrative purposes and should not be construed as limiting the scope of the present invention, and that those skilled in the art may make insubstantial modifications and adaptations to the invention described above.
Example (b):
1. the components of the formula of the special embedding material for oral cavity cast titanium are shown in table 1.
2. The preparation method of the special embedding material for oral cavity titanium casting comprises the following steps:
weighing the raw materials in the specification and the weight in the table 1, adding the raw materials into a ball mill, grinding and mixing the raw materials uniformly, and preparing the oral cavity titanium casting special embedding material according to the proportion of the powder and the mixing liquid in the table 1.
3. The application of the special embedding material for oral cavity titanium casting comprises the following steps:
uniformly mixing the embedding material according to the proportion of powder to mixing liquid of 100: 20-40, embedding a casting mold, taking down a casting ring after the embedding material is solidified and hardened, and sintering the casting mold in an automatic oven special for titanium casting, wherein the baking procedure of the casting mold is as follows: raising the temperature from room temperature to 120-160 ℃ for 60-100 min, raising the temperature to 700-850 ℃ for 80-100 min, continuing raising the temperature to 1100-1250 ℃ for 1-3 h, then slowly lowering the temperature to 600-800 ℃, wherein the raising and lowering speed is about 5 ℃/min, after 10-12 h, placing the casting mold with the constant temperature of 600-800 ℃ into a titanium casting machine for casting without a ring, quenching the cast casting mold in cold water, removing the embedding material on the surface of the casting, and performing sand blasting treatment to obtain the required casting.
Table 1 formulation components of oral titanium-casting specialized embedding materials. Particle size of raw materialParts by weight
1# 2# 3#Al2O30.8～180μm 30 40 50MgO 5～15μm 50 35 30Mg(H2PO4)2·2HO250～90μm 5 10 8NH4H2PO450～90μm 8 6 8Zr 50～90μm 1 4.5 2AlF3The mixing solution of 50-90 μm 64.52 is prepared by mixing silica sol, water and ethyl acetate powder according to the ratio of 100: 25100: 30100: 35
Claims (3)
1. The special embedding material for oral titanium casting is characterized in that the formula components (by weight) of the embedding material are as follows:
Al2O320 to 70 portions of
15-60 parts of MgO
Mg(H2PO4)2·2HO23 to 15 portions of
NH4H2PO41 to 10 parts of
1-10 parts of Zr
AlF31 to 10 parts of
The powder and the mixing liquid are 100: 20-40
Wherein the mixing solution is at least one of water, silica sol and/or ethyl acetate.
2. The method for preparing the special embedding material for oral cavity cast titanium according to claim 1, is characterized in that:
al with a particle size of 0.8 to 180 μm2O320 to 70 parts of MgO15 to 60 parts with a particle size of 5 to 15 μm and Mg (H) with a particle size of 50 to 90 μm2PO4)2·2HO23 to 15 parts of NH4H2PO41-10 parts of metal zirconium powder, 1-10 parts of AlF31-10 parts of the raw materials are added into a ball mill to be ground and mixed uniformly for later use.
3. The use of the special embedding material for oral cavity cast titanium according to claim 1 or 2, is characterized in that:
uniformly mixing the embedding material according to the proportion of powder to mixing liquid of 100: 20-40, embedding a casting mold, taking down a casting ring after the embedding material is solidified and hardened, and sintering the casting mold in an automatic oven special for titanium casting, wherein the baking procedure of the casting mold is as follows: raising the temperature from room temperature to 120-160 ℃ for 60-100 min, raising the temperature to 700-850 ℃ for 80-100 min, continuing raising the temperature to 1100-1250 ℃ for 1-3 h, then slowly lowering the temperature to 600-800 ℃, wherein the raising and lowering speed is about 5 ℃/min, after 10-12 h, placing the casting mold with the constant temperature of 600-800 ℃ into a titanium casting machine for casting without a ring, quenching the cast casting mold in cold water, removing the embedding material on the surface of the casting, and performing sand blasting treatment to obtain the required casting.
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