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The present invention belongs to the technical field of metal porcelain, and particularly relates to a metal porcelain dental crown and a preparation method.

Background technology:

According to statistics, nearly 900 million people in my country suffer from gingivitis and periodontitis. With the gradual improvement of people's medical skills and the enhancement of patients' awareness of treatment, dental clinical and scientific research have developed rapidly, and the application of metal-ceramic teeth has become more and more widespread. Metal porcelain teeth are oral restorations formed by fusing porcelain powder to a composite material substrate at high temperatures. Porcelain teeth are coated with a layer of glaze material on the inner crown of metal teeth, and the glaze is made through high-temperature calcining. The raw material is melted to form a restoration that is similar to the color and luster of real teeth. It has the characteristics of high strength, good toughness, strong corrosion resistance and good biocompatibility.

Metal porcelain dental crowns are classified according to different uses and preparation processes, mainly including gold alloy, stainless steel, nickel-chromium alloy, cobalt-chromium alloy, etc. Gold alloys are expensive, and the remaining alloys contain nickel, chromium, cobalt and other elements that are harmful to the human body to varying degrees, which can easily cause allergies and black lines in the gums. Therefore, stainless steel, nickel-chromium alloy, cobalt-chromium alloy and other porcelain tiles Dental crowns have gradually withdrawn from the market. Compared with these materials, titanium alloy materials have the advantages of high specific strength, low elastic modulus, corrosion resistance, etc., so they have gradually received widespread attention and research. However, titanium alloys have the following shortcomings as metal-ceramic dental crowns: ① The bond between gold and porcelain is poor, and porcelain chipping is prone to occur; ② The number and types of bacteria in the oral cavity are diverse, and commonly used titanium alloys have no antibacterial effect; ③ Poor biocompatibility.

The domestic patent application number is 201610967676.7, which provides a metal-ceramic restoration inner crown and its preparation method. The titanium alloy inner crown is coated with a TiN film through sputtering, which avoids the exposure of the metal color and improves the quality of the inner crown. The later porcelain process improved the bonding strength of gold and porcelain, but did not solve the problems of antibacterial properties and biocompatibility.

Technical implementation elements:

In order to solve the above problems, the present invention provides metal porcelain dental crowns and preparation methods, which can solve the following problems: ① Improve the quality of dental crowns and dental ceramics Excellent gold-porcelain bonding strength; ② Has a certain antibacterial effect; ③ Good biocompatibility.

Based on the above purpose, the present invention provides a metal porcelain dental crown and a preparation method, which are characterized in that: the surface of the dental crown is first immersed in silver, and then electroless Fe-plated is performed after the silver immersion treatment. Ag-Mo-B.

The present invention provides a metal-ceramic dental crown and a preparation method thereof. The preparation process is:

(1) Silver immersion treatment, including the following steps:

1) Prepare the immersion plating solution: silver nitrate 15~20g/L, thiourea 205~225g/L;

2) Use hydrochloric acid to adjust the pH value to 3.9~4.2, and ensure the temperature is 20~30 ℃;

3) Prepare the titanium alloy inner crown according to the dental model, put the inner crown into absolute ethanol for ultrasonic cleaning for 5 minutes, clean with deionized water and blow dry;

4) Place the inner crown into the prepared immersion plating solution and keep it for 1.5 to 2.2 minutes;

5) Take out the inner crown, let it air for 5 minutes and then wash it with water.

(2) Electroless plating of Fe-Ag-Mo-B, including the following steps:

1) Prepare chemical plating solution: FeSO4·7H2O 18~22g/L, KNaC4H4O6·4H2O 85~95g/L, KBH4 5~10g/L, NaOH 16~24g/L, Na2MoO4·2H2O 35~45g/L, AgNO3 8~10g/L;

2) Use ammonia to adjust the pH value The temperature is 8.8~9.2, and the temperature is 65~75℃;

3) Put the inner crown with silver-immersed surface into the prepared chemical plating solution and keep it for 10~15 minutes;

4) Take out the inner crown, let it air for 5 minutes and then wash it with water.

The metal porcelain dental crown provided by the present invention is immersed in silver, which weakens the activity of the metal dental crown and facilitates electroless plating on the surface.

The metal porcelain dental crown provided by the present invention reduces the surface stress of the metal dental crown through electroless Fe-Mo-Ag-B plating on the surface, and the surface layer contains materials with good bonding properties with ceramics. The B element makes the dental crown have good bonding with dental ceramics in the later porcelain process, increasing the bonding strength of gold and porcelain. The Fe and Mo elements can enhance the biocompatibility of the dental crown, and the Ag element imparts antibacterial function. .

Compared with the existing titanium alloy dental crowns, the present invention has the following advantages: ① The surface stress of the titanium alloy dental crowns is reduced through electroless Fe-Ag-Mo-B plating, and the surface layer contains The B element makes the bonding strength between the inner crown and the dental ceramic gold-porcelain high; ② The added Ag element is used to achieve the antibacterial effect; ③ The surface layer of the metal-ceramic dental crown contains Fe and Mo elements, which has good biocompatibility.

Detailed Embodiments

The principles and features of the present invention are described below with reference to examples. The examples listed are only used to explain the present invention and do not limit the scope of the present invention.

Example 1:

A metal porcelain dental crown and preparation method, including the following steps:

1) Immersion silver: ①Prepare immersion plating Solution: silver nitrate 15g/L, thiourea 210/L; ② Use hydrochloric acid to adjust the pH value to 4.0 and ensure the temperature is 25°C; ③ Prepare titanium alloy crowns according to the dental mold, and put the crowns into absolute ethanol for ultrasonic cleaning for 5 minutes. Wash with deionized water and blow dry; ④ Place the inner crown into the prepared immersion plating solution and keep it for 2.0 minutes; ⑤ Take out the inner crown and let it air for 5 minutes before washing with water.

2) Electroless plating Fe-Ag-Mo-B: ① Prepare the electroless plating solution: FeSO4·7H2O 19g, KNaC4H4O6·4H2O 92g, KBH4 8g, NaOH 20g, Na2MoO4·2H2O 40g, AgNO3 9g, add water to 1L; ②Adjust the pH value to 9.0 with ammonia water and ensure the temperature is 65℃; ③Put the inner crown with surface immersed in silver into the prepared chemical plating solution and keep it for 15 minutes; ④Take out the inner crown and let it air for 5 minutes before washing with water .

3) Antibacterial test: The prepared metal-ceramic dental crowns were ultrasonically cleaned with absolute ethanol and deionized water for 8 minutes each, and then placed in a 75% alcohol solution for 45 minutes. The test bacteria were Staphylococcus aureus and Porphyromonas gingivalis. First, put the sterilized metal-ceramic dental crown into a petri dish, add 50 mL of bacterial suspension, and incubate statically for 2 hours to allow the bacteria to fully adhere. Then use PBS solution to rinse away loose and adherent bacteria on the surface, 3 times a day. Put the rinsed metal-ceramic dental crown into 50 mL of PBS solution and oscillate ultrasonically for 3 minutes to rinse away the bacteria adhering to the surface. Then, take 5 mL of the PBS solution containing surface-adherent bacteria and spread it evenly on the culture plate. Place the culture plate into a constant-temperature incubator at 37°C and incubate for 12 hours. Observe and count the number of colonies.

4) Biocompatibility experiment: Neonatal rat skull osteoblasts were inoculated on the flat surface of the metal-ceramic dental crown. The inoculation density was 300 cells/mm2, and cells containing 10% volume fraction were used. Culture in DMEM culture medium of newborn calf serum, change the medium every 1 day, culture for 3 days and 5 days respectively, then add 0.1 mL of MTT to each well, incubate at 37°C for 4 hours, discard the supernatant, then add 0.5 mL of DMSO to each well, and use enzyme labeling The instrument measures the absorbance at a wavelength of 490nm.

Example 2:

A metal porcelain dental crown and its preparation method, including the following steps:

1) Immersion silver: ①Prepare immersion plating Solution: silver nitrate 18g/L, thiourea 212g/L; ② Use hydrochloric acid to adjust the pH value to 4.2 and ensure the temperature is 25°C; ③ Prepare titanium alloy crowns according to the dental mold, and put the crowns into absolute ethanol for ultrasonic cleaning for 5 minutes. Wash with deionized water and blow dry; ④ Place the inner crown into the prepared immersion plating solution and keep it for 2.2 minutes; ⑤ Take out the inner crown and let it air for 5 minutes before washing with water.

2) Electroless plating Fe-Ag-Mo-B: ① Prepare the electroless plating solution: FeSO4·7H2O 21g, KNaC4H4O6·4H2O 91g, KBH4 8.5g, NaOH 21g, Na2MoO4·2H2O 45g, AgNO3 10g, Add water to 1L; ②Adjust the pH value to 9.2 with ammonia water and ensure the temperature is 70℃; ③Put the inner crown with surface immersed in silver into the prepared chemical plating solution and keep it for 12 minutes; ④Take out the inner crown and let it air for 5 minutes Wash.

3) Antibacterial experiment: Carry out according to Example 1.

4) Biocompatibility experiment: Carry out according to Example 1.

Example 3:

A metal porcelain dental crown and preparation method, including the following steps:

1) Immersion silver: ①Prepare immersion plating Solution: silver nitrate 15g/L, thiourea 205g/L; ② Use hydrochloric acid to adjust the pH value to 3.9 and ensure the temperature is 20°C; ③ Prepare titanium alloy crowns according to the dental mold, and put the crowns into absolute ethanol for ultrasonic cleaning for 5 minutes. Wash with deionized water and blow dry; ④ Place the inner crown into the prepared immersion plating solution and keep it for 1.5 minutes; ⑤ Take out the inner crown and let it air for 5 minutes before washing with water.

2) Electroless plating Fe-Ag-Mo-B: ① Prepare the electroless plating solution: FeSO4·7H2O 18g, KNaC4H4O6·4H2O 85g, KBH4 5~10g, NaOH 16g, Na2MoO4·2H2O 35g, AgNO3 8g , add water to 1L; ② Use ammonia to adjust the pH value to 8.8 and ensure the temperature is 75°C; ③ Put the inner crown with silver-immersed surface into the prepared chemical plating solution and keep it for 10 minutes; ④ Take out the inner crown and let it air for 5 minutes After washing.

3) Antibacterial experiment: Carry out according to Example 1.

4) Biocompatibility experiment: Carry out according to Example 1.

Comparative Example 1:

A metal-ceramic dental crown and its preparation method, including the following steps:

1) Electroless Fe-Ag-Mo plating -B: ① Prepare chemical plating solution: FeSO4·7H2O 18g, KNaC4H4O6·4H2O 85g, KBH4 5~10g, NaOH 16g, Na2MoO4·2H2O 40g, AgNO3 9g, add water to 1L; ② Use ammonia to adjust the pH value to 8.8 and ensure the temperature 75℃; ③ Place the inner crown with surface immersed in silver into the prepared chemical plating solution and keep it for 10 minutes; ④ Take out the inner crown and let it air for 5 minutes before washing with water.

2) Antibacterial experiment: Carry out according to Example 1.

3) Biocompatibility experiment: Carry out according to Example 1.

Comparative Example 2:

A metal porcelain dental crown and a preparation method, including the following steps:

1) Preparing a titanium alloy crown.

2) Antibacterial experiment: Carry out according to Example 1.

3) Biocompatibility experiment: Carry out according to Example 1.

The results obtained in the Examples and Comparative Examples are shown in Table 1.

Table 1

The examples and comparative examples in Table 1 show that: ① In Examples 1 to 3, the titanium alloy inner crown is immersed in silver and then electrolessly plated with Fe-Ag-Mo- B reduces the surface stress of the titanium alloy inner crown, and the surface layer contains B elements that have good bonding with ceramics, so that the dental inner crown has good bonding with dental ceramics in the later porcelain process, and increases the bonding strength of gold and porcelain. In Comparative Example 1, there is no immersion silver but direct electroless plating of Fe-Ag-Mo-B. The gold-ceramic bonding strength is greatly reduced, indicating that there is no immersion silver but direct electroless plating of Fe-Ag-Mo-B. The bonding force is weak. Comparative Example 1 2 is a general titanium alloy inner crown, and the gold-ceramic bonding strength is lower; ② Except for Comparative Example 2, which does not have electroless Fe-Ag-Mo-B plating, the other 4 cases all have good antibacterial effects and biocompatibility. It shows that the Ag element imparts antibacterial function, and the Fe and Mo elements can enhance the biocompatibility of the dental crown.

The above embodiments are only for illustrating the technical concepts and characteristics of the present invention. Their purpose is to enable those familiar with this technology to understand the content of the present invention and implement it accordingly. They are not intended to limit the scope of the present invention. scope of protection. All equivalent changes or modifications made based on the spirit and essence of the present invention should be included in the protection scope of the present invention.