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CN112142462B - A kind of manufacturing method of anti-inflammatory dental restoration material with layer-by-layer self-assembled coating - Google Patents

A kind of manufacturing method of anti-inflammatory dental restoration material with layer-by-layer self-assembled coating Download PDF

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CN112142462B
CN112142462B CN202010908518.0A CN202010908518A CN112142462B CN 112142462 B CN112142462 B CN 112142462B CN 202010908518 A CN202010908518 A CN 202010908518A CN 112142462 B CN112142462 B CN 112142462B
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deionized water
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CN112142462A (en
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李国晶
赵化启
杨婷婷
杨涵崧
刘文斌
焦玉凤
王晶彦
何丽丽
姚潍
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Jiamusi University
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Abstract

一种具有层层自组装涂层的抗炎牙齿修复材料的制造方法，它涉及牙齿修复材料的制造方法。本发明的目的是要解决现有氧化锆陶瓷的脆性大，断裂韧性小，作为牙齿修复材料易发生断裂、崩瓷和不具有抗炎性的问题。方法：一、制备溶液A；二、制备浆料；三、制备瓷块；四、烧结；五、层层自组装，得到具有层层自组装涂层的抗炎牙齿修复材料。本发明制备的具有层层自组装涂层的抗炎牙齿修复材料的断裂韧性较氧化锆陶瓷提高了1倍～1.5倍。本发明可获得一种具有层层自组装涂层的抗炎牙齿修复材料。

Figure 202010908518

A method for manufacturing an anti-inflammatory dental restoration material with layers of self-assembled coatings relates to a manufacturing method for a dental restoration material. The purpose of the present invention is to solve the problems that the existing zirconia ceramics have high brittleness and low fracture toughness, and are prone to fracture, chipping and no anti-inflammatory properties as tooth restoration materials. Methods: 1. Prepare solution A; 2. Prepare slurry; 3. Prepare ceramic block; 4. Sinter; The fracture toughness of the anti-inflammatory tooth repair material with layers of self-assembled coatings prepared by the invention is improved by 1 to 1.5 times compared with zirconia ceramics. The present invention can obtain an anti-inflammatory dental restoration material with layers of self-assembled coatings.

Figure 202010908518

Description

Method for manufacturing anti-inflammatory tooth restoration material with layer-by-layer self-assembly coating
Technical Field
The present invention relates to a method for producing a dental restorative material.
Background
Teeth are a structure found in many vertebrates, the organs through which humans and tall animals chew food. Teeth are the hardest organs of the human body. Generally, teeth are white in color and hard in texture. The various shapes of teeth are suitable for a variety of uses, including tearing, grinding food. Restorative materials are one of the key areas of research in the dental field, since restorative materials are needed once a tooth is damaged.
At present, the dental prosthetic material is gradually developed from resin in the initial stage to metal, and finally developed to a zirconia denture material, the zirconia ceramic material has good comprehensive properties such as high melting point, high hardness, high wear resistance, oxidation resistance and the like, the raw material sources for production are sufficient, the manufacturing cost is low, and the material is suitable for large-scale industrial production, so the zirconia is gradually the dental prosthetic material favored by people, and in addition, the zirconia ceramic has good biocompatibility and has glaze texture and transparency close to natural teeth of human bodies. However, the low fracture toughness and high brittleness of zirconia ceramics limit their application because of their natural brittleness, which prevents further widespread use of such products.
Therefore, there is a strong need for a dental restorative material having high bending strength, high fracture toughness, anti-inflammation, and biocompatibility, and there is no report on such a restorative material.
Disclosure of Invention
The invention aims to solve the problems that the existing zirconia ceramics have large brittleness and small fracture toughness, are easy to fracture and break porcelain and do not have anti-inflammation when being used as tooth repairing materials, and provides a method for manufacturing an anti-inflammation tooth repairing material with a layer-by-layer self-assembly coating.
A method for manufacturing an anti-inflammatory tooth restoration material with a layer-by-layer self-assembly coating is completed according to the following steps:
firstly, uniformly mixing deionized water, sodium oleate, sodium carboxymethylcellulose and polyvinyl alcohol, and stirring to obtain a solution A;
the mass ratio of the deionized water to the sodium carboxymethyl cellulose in the first step is 100 (0.3-1);
the mass ratio of the deionized water to the polyvinyl alcohol in the first step is 100 (0.5-2);
the mass ratio of the deionized water to the sodium oleate in the first step is 100 (1.5-2);
secondly, adding nano zirconia powder, nano alumina powder and nano cerium dioxide powder into the solution A, and stirring to obtain slurry;
the mass ratio of the nano zirconia powder, the nano alumina powder and the nano ceria powder in the second step is 100 (4-8) to (8-15);
the mass ratio of the solution A to the nano zirconia powder in the step two is 100 (10-20);
thirdly, carrying out spray granulation on the slurry in a spray granulator, and pressing the obtained particles to obtain a ceramic block;
the thickness of the porcelain block in the third step is 15 mm-30 mm;
the pressing pressure in the third step is 80MPa to 150 MPa;
fourthly, placing the porcelain block into a muffle furnace, heating to 250-300 ℃ at a heating rate of 2-4 ℃/min, then preserving heat at 250-300 ℃ for 2-4 h, heating from 250-300 ℃ to 750-800 ℃ at a heating rate of 2-4 ℃/min, then preserving heat at 750-800 ℃ for 2-3 h, heating from 750-800 ℃ to 1500-1560 ℃ at a heating rate of 2-4 ℃/min, and then preserving heat at 1500-1560 ℃ for 1-2 h; obtaining a composite ceramic block toughened by alumina and cerium dioxide;
fifthly, self-assembling layer by layer:
firstly, immersing the composite ceramic block toughened by the alumina and the cerium dioxide into a polyvinyl alcohol solution for 5-10 min, taking out and drying; then placing the mixture into a tannic acid solution for soaking for 5min to 10min, taking out and drying;
the volume ratio of the mass of the polyvinyl alcohol in the polyvinyl alcohol solution in the step V to the deionized water is (1 g-2 g) to 100 mL;
the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water in the step V is (1 g-2 g) to 100 mL;
fifthly, repeating the fifth step for 20-40 times to obtain a composite ceramic block coated with the coating;
thirdly, placing the composite ceramic block coated with the coating in epigallocatechin gallate solution for 5-10 min, taking out and drying, then placing the ceramic block in tannic acid solution for soaking for 5-10 min, taking out and drying;
the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water in the step five (1 g-2 g) is 100 mL;
the volume ratio of the mass of the epigallocatechin gallate in the epigallocatechin gallate solution to the deionized water is (0.001 g-0.01 g) 1 mL;
fourthly, repeating the fifth step and the third step for 20 to 40 times to obtain the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating.
The principle and the advantages of the invention are as follows:
the preparation method comprises the steps of preparing an alumina and cerium dioxide toughened composite ceramic block by using sodium oleate as a dispersing agent, sodium carboxymethylcellulose and polyvinyl alcohol as binders, nano-zirconia powder as a raw material and nano-alumina powder and nano-cerium dioxide powder as toughening agents, and preparing a high-hardness coating on the surface of the alumina and cerium dioxide toughened composite ceramic block by using polyvinyl alcohol, tannic acid and epigallocatechin gallate as raw materials through a layer-by-layer self-assembly method, wherein the coating can prevent body fluid from permeating, and has anti-inflammation and is not easy to cause inflammation due to the fact that epigallocatechin gallate is contained;
the fracture toughness of the zirconia ceramic is 8 MPa.m1/2The fracture toughness of the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating prepared by the invention can reach 16 MPa.m1/2～20MPa·m1/2Therefore, compared with zirconia ceramics, the fracture toughness of the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating prepared by the invention is improved by 1-1.5 times.
Drawings
Fig. 1 is a digital photograph of an anti-inflammatory dental restoration material with a layer-by-layer self-assembled coating prepared in example one.
Detailed Description
The first embodiment is as follows: the method for manufacturing the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating is completed according to the following steps:
firstly, uniformly mixing deionized water, sodium oleate, sodium carboxymethylcellulose and polyvinyl alcohol, and stirring to obtain a solution A;
the mass ratio of the deionized water to the sodium carboxymethyl cellulose in the first step is 100 (0.3-1);
the mass ratio of the deionized water to the polyvinyl alcohol in the first step is 100 (0.5-2);
the mass ratio of the deionized water to the sodium oleate in the first step is 100 (1.5-2);
secondly, adding nano zirconia powder, nano alumina powder and nano cerium dioxide powder into the solution A, and stirring to obtain slurry;
the mass ratio of the nano zirconia powder, the nano alumina powder and the nano ceria powder in the second step is 100 (4-8) to (8-15);
the mass ratio of the solution A to the nano zirconia powder in the step two is 100 (10-20);
thirdly, carrying out spray granulation on the slurry in a spray granulator, and pressing the obtained particles to obtain a ceramic block;
the thickness of the porcelain block in the third step is 15 mm-30 mm;
the pressing pressure in the third step is 80MPa to 150 MPa;
fourthly, placing the porcelain block into a muffle furnace, heating to 250-300 ℃ at a heating rate of 2-4 ℃/min, then preserving heat at 250-300 ℃ for 2-4 h, heating from 250-300 ℃ to 750-800 ℃ at a heating rate of 2-4 ℃/min, then preserving heat at 750-800 ℃ for 2-3 h, heating from 750-800 ℃ to 1500-1560 ℃ at a heating rate of 2-4 ℃/min, and then preserving heat at 1500-1560 ℃ for 1-2 h; obtaining a composite ceramic block toughened by alumina and cerium dioxide;
fifthly, self-assembling layer by layer:
firstly, immersing the composite ceramic block toughened by the alumina and the cerium dioxide into a polyvinyl alcohol solution for 5-10 min, taking out and drying; then placing the mixture into a tannic acid solution for soaking for 5min to 10min, taking out and drying;
the volume ratio of the mass of the polyvinyl alcohol in the polyvinyl alcohol solution in the step V to the deionized water is (1 g-2 g) to 100 mL;
the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water in the step V is (1 g-2 g) to 100 mL;
fifthly, repeating the fifth step for 20-40 times to obtain a composite ceramic block coated with the coating;
thirdly, placing the composite ceramic block coated with the coating in epigallocatechin gallate solution for 5-10 min, taking out and drying, then placing the ceramic block in tannic acid solution for soaking for 5-10 min, taking out and drying;
the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water in the step five (1 g-2 g) is 100 mL;
the volume ratio of the mass of the epigallocatechin gallate in the epigallocatechin gallate solution to the deionized water is (0.001 g-0.01 g) 1 mL;
fourthly, repeating the fifth step and the third step for 20 to 40 times to obtain the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating.
The second embodiment is as follows: the present embodiment differs from the present embodiment in that: the grain diameter of the nano zirconia powder in the second step is 20 nm-40 nm. Other steps are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the grain size of the nano alumina powder in the second step is 40 nm-60 nm. The other steps are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is as follows: the particle size of the nano cerium dioxide powder in the second step is 40 nm-60 nm. The other steps are the same as those in the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the particle size of the particles obtained by spray granulation in the third step is 10-30 μm. The other steps are the same as those in the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is as follows: the atomization frequency of the spray granulation in the third step is 200Hz, the rotating speed of a feed pump is 30r/min, and the drying temperature is 220-300 ℃. The other steps are the same as those in the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the pressing pressure in the third step is 80MPa to 100 MPa. The other steps are the same as those in the first to sixth embodiments.
The specific implementation mode is eight: the difference between this embodiment and one of the first to seventh embodiments is: putting the porcelain block into a muffle furnace, heating to 280 ℃ at the heating rate of 3 ℃/min, then preserving heat for 3h at 280 ℃, heating from 280 ℃ to 800 ℃ at the heating rate of 3 ℃/min, then preserving heat for 2h at 800 ℃, heating from 800 ℃ to 1550 ℃ at the heating rate of 3 ℃/min, and then preserving heat for 1.5h at 1550 ℃; and obtaining the composite ceramic block. The other steps are the same as those in the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: fifthly, repeating the fifth step for 30-40 times to obtain the composite ceramic block coated with the coating; and in the step V, repeating the step V and the step V for 30 to 40 times to obtain the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating. The other steps are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the difference between this embodiment and one of the first to ninth embodiments is as follows: the volume ratio of the weight of the epigallocatechin gallate in the epigallocatechin gallate solution to the deionized water is (0.005 g-0.008 g):1 mL. The other steps are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows: a method for manufacturing an anti-inflammatory tooth restoration material with a layer-by-layer self-assembly coating is completed according to the following steps:
firstly, uniformly mixing deionized water, sodium oleate, sodium carboxymethylcellulose and polyvinyl alcohol, and stirring to obtain a solution A;
the mass ratio of the deionized water to the sodium carboxymethyl cellulose in the first step is 100: 0.6;
the mass ratio of the deionized water to the polyvinyl alcohol in the first step is 100: 1.2;
the mass ratio of the deionized water to the sodium oleate in the step one is 100: 1.8;
secondly, adding nano zirconia powder, nano alumina powder and nano cerium dioxide powder into the solution A, and stirring to obtain slurry;
the grain diameter of the nano zirconia powder in the step two is 20 nm-40 nm;
the grain size of the nano alumina powder in the second step is 40 nm-60 nm;
the particle size of the nano cerium dioxide powder in the second step is 40 nm-60 nm;
the mass ratio of the nano zirconia powder, the nano alumina powder and the nano ceria powder in the step two is 100:6: 10;
the mass ratio of the solution A to the nano zirconia powder in the step two is 100: 15;
thirdly, carrying out spray granulation on the slurry in a spray granulator, and pressing the obtained particles to obtain a ceramic block;
the particle size of the particles obtained by spray granulation in the third step is 10-15 mu m;
the thickness of the porcelain block in the third step is 20 mm;
the atomization frequency of the spray granulation in the third step is 200Hz, the rotating speed of a feed pump is 30r/min, and the drying temperature is 300 ℃;
the pressing pressure in the third step is 90 MPa;
fourthly, placing the porcelain block into a muffle furnace, heating to 280 ℃ at a heating rate of 3 ℃/min, then preserving heat at 280 ℃ for 3h, heating from 280 ℃ to 800 ℃ at a heating rate of 3 ℃/min, then preserving heat at 800 ℃ for 2h, heating from 800 ℃ to 1550 ℃ at a heating rate of 3 ℃/min, and then preserving heat at 1550 ℃ for 1.5 h; obtaining a composite ceramic block toughened by alumina and cerium dioxide;
fifthly, self-assembling layer by layer:
firstly, immersing the alumina and cerium dioxide toughened composite ceramic block into a polyvinyl alcohol solution for 10min, taking out and drying; then soaking in tannic acid solution for 10min, taking out and drying;
the volume ratio of the mass of the polyvinyl alcohol in the polyvinyl alcohol solution in the fifth step to the deionized water is 1.5g:100 mL;
fifthly, the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water is 1.5g to 100 mL;
fifthly, repeating the step five and the step 30 times to obtain a composite ceramic block coated with the coating;
thirdly, placing the composite ceramic block coated with the coating in epigallocatechin gallate solution for 10min, taking out and drying, then placing the ceramic block in tannic acid solution for 10min, taking out and drying;
the volume ratio of the mass of the epigallocatechin gallate in the epigallocatechin gallate solution in the fifth step to the deionized water is 0.006g:1 mL;
fifthly, the volume ratio of the mass of the tannic acid in the tannic acid solution to the deionized water is 1.5g to 100 mL;
fourthly, repeating the fifth step and the third step for 30 times to obtain the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating.
Example one prepared anti-inflammatory dental restoration material with a layer-by-layer self-assembled coating has a fracture toughness of up to 20MPa · m1/2。
Example two: the present embodiment is different from the first embodiment in that: and the mass ratio of the nano zirconia powder, the nano alumina powder and the nano ceria powder in the step two is 100:4: 8. Other steps and parameters are the same as those in the first embodiment.
The fracture toughness of the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating prepared in the second embodiment can reach 16.9 MPa.m1/2。
Example three: the present embodiment is different from the first embodiment in that: in the fourth step, the porcelain block is put into a muffle furnace, the temperature is raised to 250 ℃ at the heating rate of 4 ℃/min, then the heat is preserved for 2h at 250 ℃, the temperature is raised from 250 ℃ to 780 ℃ at the heating rate of 4 ℃/min, then the heat is preserved for 3h at 780 ℃, the temperature is raised from 780 ℃ to 1500 ℃ at the heating rate of 4 ℃/min, and then the heat is preserved for 2h at 1500 ℃. And obtaining the alumina and cerium dioxide toughened composite ceramic block. Other steps and parameters are the same as those in the first embodiment.
The fracture toughness of the anti-inflammatory tooth restoration material with the layer-by-layer self-assembly coating prepared in the third embodiment can reach 18.3 MPa.m1/2。
Comparative example: the zirconia ceramic is prepared by the following steps:
firstly, adding nano zirconia powder into deionized water, and stirring to obtain slurry;
the particle size of the nano zirconia powder in the step one is 20 nm-40 nm;
the mass ratio of the deionized water to the nano zirconia powder in the first step is 100: 15;
secondly, carrying out spray granulation on the slurry in a spray granulator, and pressing the obtained particles to obtain a ceramic block;
the particle size of the particles obtained by spray granulation in the second step is 10-15 μm;
the thickness of the porcelain block in the second step is 20 mm;
the atomization frequency of the spray granulation in the step two is 200Hz, the rotating speed of a feed pump is 30r/min, and the drying temperature is 300 ℃;
the pressing pressure in the step two is 90 MPa;
thirdly, placing the porcelain block into a muffle furnace, heating to 280 ℃ at a heating rate of 3 ℃/min, then preserving heat at 280 ℃ for 3h, heating from 280 ℃ to 800 ℃ at a heating rate of 3 ℃/min, then preserving heat at 800 ℃ for 2h, heating from 800 ℃ to 1550 ℃ at a heating rate of 3 ℃/min, and then preserving heat at 1550 ℃ for 1.5 h; obtaining the zirconia ceramics.
The fracture toughness of the zirconia ceramics prepared by the comparative example can reach 8 MPa.m1/2。
Fig. 1 is a digital photograph of an anti-inflammatory dental restoration material with a layer-by-layer self-assembled coating prepared in example one.
The anti-inflammatory dental restoration materials having layer-by-layer self-assembled coatings prepared in examples one, two and three did not cause oral inflammation as dental restoration materials.
The thicknesses of the anti-inflammatory dental restoration materials having a layer-by-layer self-assembled coating prepared in examples one, two and three as dental restorations are listed in table 1.
TABLE 1
Examples Thickness/mm
Example one 0.29mm～0.64mm
Example two 0.33mm～0.82mm
EXAMPLE III 0.32mm～0.79mm

Claims (1)

1.一种具有层层自组装涂层的抗炎牙齿修复材料的制造方法，其特征在于该制造方法是按以下步骤完成的：1. a manufacture method of the anti-inflammatory dental restoration material with layer by layer self-assembly coating, it is characterized in that this manufacture method is completed according to the following steps: 一、将去离子水、油酸钠、羧甲基纤维素钠和聚乙烯醇混合均匀，再进行搅拌，得到溶液A；1. Mix the deionized water, sodium oleate, sodium carboxymethyl cellulose and polyvinyl alcohol uniformly, and then stir to obtain solution A; 步骤一中所述的去离子水与羧甲基纤维素钠的质量比为100:0.6；The mass ratio of deionized water described in step 1 and sodium carboxymethyl cellulose is 100:0.6; 步骤一中所述的去离子水与聚乙烯醇的质量比为100:1.2；The mass ratio of deionized water described in step 1 and polyvinyl alcohol is 100:1.2; 步骤一中所述的去离子水与油酸钠的质量比为100:1.8；The mass ratio of deionized water described in step 1 and sodium oleate is 100:1.8; 二、向溶液A中加入纳米氧化锆粉末、纳米氧化铝粉末和纳米二氧化铈粉末，再进行搅拌，得到浆料；2. Add nano-zirconia powder, nano-alumina powder and nano-ceria powder to solution A, and then stir to obtain slurry; 步骤二中所述的纳米氧化锆粉末的粒径为20nm~40nm；The particle size of the nano-zirconia powder described in step 2 is 20nm～40nm; 步骤二中所述的纳米氧化铝粉末的粒径为40nm~60nm；The particle size of the nano-alumina powder described in step 2 is 40nm～60nm; 步骤二中所述的纳米二氧化铈粉末的粒径为40nm~60nm；The particle size of the nano-ceria powder described in step 2 is 40nm～60nm; 步骤二中所述的纳米氧化锆粉末、纳米氧化铝粉末和纳米二氧化铈粉末的质量比为100:6:10；The mass ratio of the nano-zirconia powder, nano-alumina powder and nano-ceria powder described in step 2 is 100:6:10; 步骤二中所述的溶液A与纳米氧化锆粉末的质量比为100:15；The mass ratio of solution A described in step 2 and nano-zirconia powder is 100:15; 三、将浆料在喷雾造粒机中进行喷雾造粒，得到的颗粒再进行压制，得到瓷块；3. The slurry is spray granulated in a spray granulator, and the obtained granules are pressed again to obtain a porcelain block; 步骤三中喷雾造粒得到的颗粒粒径为10μm~15μm；The particle size obtained by spray granulation in step 3 is 10 μm~15 μm; 步骤三中所述的瓷块的厚度为20mm；The thickness of the porcelain block described in step 3 is 20mm; 步骤三中所述的喷雾造粒的雾化频率为200Hz，进料泵转速为30r/min，干燥温度为300℃；The atomization frequency of the spray granulation described in step 3 is 200Hz, the rotational speed of the feed pump is 30r/min, and the drying temperature is 300°C; 步骤三中所述的压制的压力为90MPa；The pressure of the pressing described in the step 3 is 90MPa; 四、将瓷块放入马弗炉中，以3℃/min的升温速率升温至280℃，再在280℃下保温3h，再以3℃/min的升温速率从280℃升温至800℃，再在800℃下保温2h，再以3℃/min的升温速率从800℃升温至1550℃，再在1550℃下保温1.5h；得到氧化铝和二氧化铈增韧的复合陶瓷块；4. Put the porcelain block into the muffle furnace, heat it up to 280°C at a heating rate of 3°C/min, keep it at 280°C for 3 hours, and then heat it up from 280°C to 800°C at a heating rate of 3°C/min. The temperature was kept at 800 °C for 2 h, then increased from 800 °C to 1550 °C at a heating rate of 3 °C/min, and then kept at 1550 °C for 1.5 h; the composite ceramic block toughened by alumina and ceria was obtained; 五、层层自组装：5. Layer-by-layer self-assembly: ①、将氧化铝和二氧化铈增韧的复合陶瓷块浸入到聚乙烯醇溶液中10min，取出后吹干；然后置于单宁酸溶液中浸泡10min，取出后吹干；1. Immerse the alumina and ceria toughened composite ceramic block in polyvinyl alcohol solution for 10min, take it out and blow dry; then place it in tannic acid solution for 10 minutes, take out and blow dry; 步骤五①中所述的聚乙烯醇溶液中聚乙烯醇的质量与去离子水的体积比为1.5g:100mL；The mass ratio of polyvinyl alcohol to deionized water in the polyvinyl alcohol solution described in step 5. is 1.5g:100mL; 步骤五①中所述的单宁酸溶液中单宁酸的质量与去离子水的体积比为1.5g:100mL；The mass ratio of tannic acid in the tannic acid solution described in step 5. to deionized water is 1.5g:100mL; ②、重复步骤五①30次，得到涂覆有涂层的复合陶瓷块；②, repeat step 5 ① 30 times to obtain a composite ceramic block coated with a coating; ③、将涂覆有涂层的复合陶瓷块置于表没食子儿茶素没食子酸酯溶液中10min，取出后吹干，然后置于单宁酸溶液中浸泡10min，取出后吹干；3. Place the coated composite ceramic block in the epigallocatechin gallate solution for 10min, take it out and dry it, then place it in the tannic acid solution and soak it for 10min, take it out and dry it; 步骤五③中所述的表没食子儿茶素没食子酸酯溶液中表没食子儿茶素没食子酸酯的质量与去离子水的体积比为0.006g:1mL；The mass ratio of epigallocatechin gallate and deionized water in the epigallocatechin gallate solution described in step 5 3. is 0.006g:1mL; 步骤五③中所述的单宁酸溶液中单宁酸的质量与去离子水的体积比为1.5g:100mL；In the tannic acid solution described in step 5., the mass ratio of tannic acid and deionized water is 1.5g:100mL; ④、重复步骤五③30次，得到具有层层自组装涂层的抗炎牙齿修复材料；④, repeat step 5 ③ 30 times to obtain anti-inflammatory dental restoration material with layers of self-assembled coatings; 步骤五④中所述的具有层层自组装涂层的抗炎牙齿修复材料中具有层层自组装涂层能够防止体液渗透。The layer-by-layer self-assembled coating layer in the anti-inflammatory dental restoration material with layer-by-layer self-assembled coating described in step 5 (4) can prevent the penetration of body fluids.
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