CN109044548B - Metal ceramic tooth inner crown and preparation method thereof - Google Patents

Metal ceramic tooth inner crown and preparation method thereof Download PDF

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Publication number
CN109044548B
CN109044548B CN201810726135.4A CN201810726135A CN109044548B CN 109044548 B CN109044548 B CN 109044548B CN 201810726135 A CN201810726135 A CN 201810726135A CN 109044548 B CN109044548 B CN 109044548B
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inner crown
coping
silver
metal
tooth
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CN109044548A (en
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贾占奎
金志波
孙科
李松超
姚文诚
杨锦建
丁亚飞
郝钢
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First Affiliated Hospital of Zhengzhou University
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A61C13/083—Porcelain or ceramic teeth
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/0003—Making bridge-work, inlays, implants or the like
    • A61C13/0006—Production methods
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/31—Coating with metals
    • C23C18/42—Coating with noble metals
    • C23C18/44—Coating with noble metals using reducing agents
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
    • C23C18/48—Coating with alloys
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
    • C23C28/021—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material including at least one metal alloy layer
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C2201/00—Material properties

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • General Chemical & Material Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Epidemiology (AREA)
  • Oral & Maxillofacial Surgery (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Dental Preparations (AREA)
  • Dental Prosthetics (AREA)

Abstract

The invention provides a metal ceramic tooth coping and a preparation method thereof. The metal tooth inner crown is treated by silver immersion, so that the activity of metal is weakened, and chemical plating on the surface is facilitated; after the chemical plating of Fe-Mo-Ag-B, the surface stress of the metal inner crown is reduced, and the surface layer contains B elements with good binding property with ceramics, so that the metal inner crown has good binding property with dental ceramics in the later porcelain baking process, the binding strength of the golden porcelain is increased, the Fe and Mo elements can enhance the biocompatibility of the metal inner crown, and the Ag element has an antibacterial function.

Description

Metal ceramic tooth inner crown and preparation method thereof
Technical Field
The invention belongs to the technical field of metal porcelain, and particularly relates to a metal porcelain tooth inner crown and a preparation method thereof.
Background
According to statistics, nearly 9 hundred million people in China have gingivitis and periodontitis. With the gradual improvement of the level of people and the enhancement of the treatment consciousness of patients, the clinical dentistry and scientific research are rapidly developed, and the application of the metal porcelain tooth is more and more extensive. The metal porcelain tooth is a dental restoration formed by fusing porcelain powder on a composite material substrate at high temperature, namely, a layer of glaze material is coated on the inner crown of the metal tooth, and the glaze material is fused to form the restoration with the color and luster similar to that of a real tooth through high-temperature calcination.
The metal porcelain tooth inner crown mainly comprises gold alloy, stainless steel, nickel-chromium alloy, cobalt-chromium alloy and the like according to different classifications of using and preparing processes, the gold alloy is expensive, and other alloys contain elements harmful to human bodies, such as nickel, chromium, cobalt and the like, in different degrees, so that allergy is easy to occur to patients and a black line phenomenon appears on gum, so that the porcelain tooth inner crowns of stainless steel, nickel-chromium alloy, cobalt-chromium alloy and the like gradually quit the market.
The domestic patent application number 201610967676.7 provides a metal porcelain restoration inner crown and a preparation method thereof, a TiN film is plated on the titanium alloy inner crown in a sputtering mode, the exposure of metal color is avoided, the gold and porcelain bonding strength in the later porcelain baking process is improved, and the problems of antibacterial property and biocompatibility are not solved.
Disclosure of Invention
In order to solve the problems, the invention provides a metal ceramic dental coping and a preparation method thereof, and can solve the problems that ① improves the bonding strength of the dental coping and the golden porcelain of dental ceramics, ② has a certain antibacterial effect, and ③ has good biocompatibility.
Based on the above purposes, the invention provides a metal porcelain tooth coping and a preparation method thereof, which are characterized in that: the surface of the inner crown of the tooth is firstly soaked with silver and then chemically plated with Fe-Ag-Mo-B after the silver soaking treatment.
The invention provides a baked metal porcelain tooth coping and a preparation method thereof, and the preparation process comprises the following steps:
(1) the silver immersion treatment comprises the following steps:
1) preparing immersion plating solution comprising 15-20 g/L g of silver nitrate and 205-225 g/L g of thiourea;
2) adjusting the pH value to 3.9-4.2 by hydrochloric acid, and ensuring the temperature to be 20-30 ℃;
3) preparing a titanium alloy inner crown according to a tooth mould, putting the inner crown into absolute ethyl alcohol for ultrasonic cleaning for 5min, cleaning with deionized water, and drying;
4) placing the inner crown into the prepared dip-plating solution for 1.5-2.2 min;
5) taking out the inner crown, air-drying in air for 5min, and washing with water.
(2) The chemical plating of Fe-Ag-Mo-B comprises the following steps:
1) preparing a chemical plating solution: FeSO4·7H2O 18～22g/L，KNaC4H4O6·4H2O 85～95g/L，KBH45～10g/L，NaOH 16～24g/L，Na2MoO4·2H2O 35～45g/L，AgNO38～10g/L；
2) Adjusting the pH value to 8.8-9.2 by using ammonia water, and adjusting the temperature to 65-75 ℃;
3) placing the inner crown with the surface soaked with silver into the prepared chemical plating solution for 10-15 min;
4) taking out the inner crown, air-drying in air for 5min, and washing with water.
The metal porcelain tooth coping provided by the invention is subjected to silver immersion treatment, so that the activity of the metal tooth coping is weakened, and the chemical plating on the surface is facilitated.
The metal porcelain tooth inner crown reduces the surface stress of the metal tooth inner crown by chemically plating Fe-Mo-Ag-B on the surface, and the surface layer contains B elements with good bonding property with ceramics, so that the tooth inner crown has good bonding property with dental ceramics in the later porcelain-firing process, the bonding strength of the porcelain is increased, the Fe and Mo elements can enhance the biocompatibility of the tooth inner crown, and the Ag element has an antibacterial function.
Compared with the existing titanium alloy dental coping, the titanium alloy dental coping has the advantages that ① reduces the surface stress of the titanium alloy dental coping through chemical plating of Fe-Ag-Mo-B, the surface layer contains B elements, so that the bonding strength of the dental coping and the gold and porcelain of dental ceramics is high, ② achieves an antibacterial effect by utilizing the added Ag elements, and the ③ metal porcelain dental coping has good biocompatibility because the surface layer contains Fe and Mo elements.
Detailed Description
The principles and features of this invention are described below in conjunction with embodiments, which are set forth merely to illustrate the invention and are not intended to limit the scope of the invention.
Example 1:
a metal porcelain tooth coping and a preparation method thereof comprise the following steps:
1) the method comprises the steps of preparing a silver dipping solution from ①, wherein the silver dipping solution comprises 15 g/L of silver nitrate and 210/L of thiourea, adjusting the pH value of ② to 4.0 by hydrochloric acid, ensuring the temperature to be 25 ℃, preparing a titanium alloy coping ③ according to a tooth model, putting the coping into absolute ethyl alcohol, performing ultrasonic cleaning for 5min, cleaning with deionized water, drying, putting ④ the coping into the prepared silver dipping solution, keeping the coping for 2.0min, taking ⑤ out the coping, airing in the air for 5min, and then performing water cleaning.
2) ① preparing chemical plating solution FeSO4·7H2O 19g，KNaC4H4O6·4H2O 92g，KBH48g，NaOH 20g，Na2MoO4·2H2O 40g，AgNO39g of water is added until the temperature is 1L, ② ammonia water is used for adjusting the pH value to 9.0 and ensuring the temperature to be 65 ℃, ③ the inner crown with the surface soaked with silver is put into prepared chemical plating solution for keeping for 15min, ④ the inner crown is taken out and aired in the air for 5min and then washed with water.
3) The antibacterial experiment comprises the steps of ultrasonically cleaning the prepared metal porcelain tooth inner crown by absolute ethyl alcohol and deionized water for 8min respectively, then placing the metal porcelain tooth inner crown into an alcohol solution with the volume fraction of 75% for disinfection for 45min, testing whether bacteria are staphylococcus aureus and porphyromonas gingivalis, firstly placing the disinfected metal porcelain tooth inner crown into a culture dish, adding 50m L bacteria suspension, standing and culturing for 2h to ensure that the bacteria are fully adhered, then washing off the loose and adhered bacteria on the surface by using a PBS solution, washing for 3 times in total, placing the washed metal porcelain tooth inner crown into a 50m L PBS solution, ultrasonically oscillating for 3min to wash off the bacteria on the surface, then taking 5m L of the PBS solution containing the adhered bacteria on the surface, uniformly paving the PBS solution on a culture substrate, placing the culture substrate into a constant-temperature culture box at 37 ℃ for culturing for 12h, observing and calculating the colony count.
4) Biocompatibility experiment: inoculating new rat skull osteoblasts on the smooth surface of the inner crown of the metal porcelain tooth, wherein the inoculation density is 300/mm2By containing volumeCulturing 10% newborn bovine serum in DMEM medium, changing culture medium every 1d, culturing for 3d and 5d, adding MTT 0.1m L into each well, culturing for 4h at 37 ℃, removing supernatant, adding DMSO 0.5m L into each well, and measuring absorbance at 490nm by using an enzyme-labeling instrument.
Example 2:
a metal porcelain tooth coping and a preparation method thereof comprise the following steps:
1) the method comprises the steps of preparing a silver dipping solution from ① g/L g of silver nitrate and 212 g/L g of thiourea, adjusting the pH value of ② to 4.2 by hydrochloric acid to ensure the temperature to be 25 ℃, preparing a titanium alloy coping ③ according to a tooth model, putting the coping into absolute ethyl alcohol, ultrasonically cleaning for 5min, cleaning with deionized water, drying, ④ putting the coping into the prepared silver dipping solution, keeping for 2.2min, ⑤ taking out the coping, airing for 5min in air, and then washing with water.
2) ① preparing chemical plating solution FeSO4·7H2O 21g，KNaC4H4O6·4H2O 91g，KBH48.5g，NaOH 21g，Na2MoO4·2H2O 45g，AgNO310g of water is added until the water content is 1L, ② ammonia water is used for adjusting the pH value to 9.2, the temperature is ensured to be 70 ℃, ③ the inner crown with the surface soaked with silver is put into prepared chemical plating solution for keeping for 12min, ④ the inner crown is taken out, aired in the air for 5min and then washed with water.
3) And (3) antibacterial experiment: the procedure is as in example 1.
4) Biocompatibility experiment: the procedure is as in example 1.
Example 3:
a metal porcelain tooth coping and a preparation method thereof comprise the following steps:
1) the method comprises the steps of ① preparing immersion plating solution, namely 15 g/L g of silver nitrate and 205 g/L g of thiourea, ② adjusting the pH value to 3.9 by hydrochloric acid to ensure the temperature to be 20 ℃, ③ preparing a titanium alloy coping according to a tooth model, putting the coping into absolute ethyl alcohol, ultrasonically cleaning for 5min, cleaning with deionized water, drying, ④ putting the coping into the prepared immersion plating solution, keeping for 1.5min, ⑤ taking out the coping, airing for 5min in air, and then washing with water.
2) ① preparing chemical plating solution FeSO4·7H2O 18g，KNaC4H4O6·4H2O 85g，KBH45～10g，NaOH 16g，Na2MoO4·2H2O 35g，AgNO38g of the crown, adding water to 1L, adjusting the pH value of ② to 8.8 by using ammonia water to ensure that the temperature is 75 ℃, ③ putting the inner crown with the surface soaked with silver into prepared chemical plating solution for keeping for 10min, ④ taking out the inner crown, airing in the air for 5min and then washing with water.
3) And (3) antibacterial experiment: the procedure is as in example 1.
4) Biocompatibility experiment: the procedure is as in example 1.
Comparative example 1:
a metal porcelain tooth coping and a preparation method thereof comprise the following steps:
1) ① preparing chemical plating solution FeSO4·7H2O 18g，KNaC4H4O6·4H2O 85g，KBH45～10g，NaOH 16g，Na2MoO4·2H2O 40g，AgNO39g of water is added until the temperature is 1L, ② ammonia water is used for adjusting the pH value to 8.8 and ensuring the temperature to be 75 ℃, ③ the inner crown with the surface soaked with silver is put into prepared chemical plating solution for keeping for 10min, ④ the inner crown is taken out and aired in the air for 5min and then washed with water.
2) And (3) antibacterial experiment: the procedure is as in example 1.
3) Biocompatibility experiment: the procedure is as in example 1.
Comparative example 2:
a metal porcelain tooth coping and a preparation method thereof comprise the following steps:
1) and preparing the titanium alloy coping.
2) And (3) antibacterial experiment: the procedure is as in example 1.
3) Biocompatibility experiment: the procedure is as in example 1.
The results obtained for the examples and comparative examples are shown in table 1.
TABLE 1
Figure BDA0001719773740000041
The examples and the comparative examples in Table 1 show that ① the titanium alloy coping in examples 1-3 has reduced the surface stress of the titanium alloy coping by immersing in silver and then chemically plating Fe-Ag-Mo-B, and the surface layer contains B element with good bonding property with ceramic, so that the dental coping has good bonding property with dental ceramic in the later porcelain baking process, and the bonding strength of the porcelain is increased, the comparative example 1 is not immersed in silver but directly chemically plated with Fe-Ag-Mo-B, the bonding strength of the porcelain is greatly reduced, which indicates that the immersion in silver but directly chemically plated with Fe-Ag-Mo-B is weak, the comparative example 2 is a general titanium alloy coping, and the bonding strength of the porcelain is lower, ② other 4 examples except the comparative example 2 without chemically plated with Fe-Ag-Mo-B all have better antibacterial effect and biocompatibility, which indicates that the Ag element has an antibacterial function, and the Fe and Mo element can enhance the biocompatibility of the dental coping.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (2)

1. A preparation method of a metal porcelain tooth coping is characterized in that the surface of a titanium alloy tooth coping is firstly soaked with silver, and then is chemically plated with Fe-Ag-Mo-B after the silver soaking treatment;
the silver leaching process comprises the following steps:
1) preparing immersion plating solution comprising 15-20 g/L g of silver nitrate and 205-225 g/L g of thiourea;
2) adjusting the pH value to 3.9-4.2 by hydrochloric acid, and ensuring the temperature to be 20-30 ℃;
3) preparing a titanium alloy inner crown according to a tooth mould, putting the inner crown into absolute ethyl alcohol for ultrasonic cleaning for 5min, cleaning with deionized water, and drying;
4) placing the inner crown into the prepared dip-plating solution for 1.5-2.2 min;
5) taking out the inner crown, airing in air for 5min, and washing with water;
the chemical Fe-Ag-Mo-B plating process comprises the following steps:
1) preparation ofChemical plating solution: FeSO4·7H2O 18～22g/L，KNaC4H4O6·4H2O 85～95g/L，KBH45～10g/L，NaOH 16～24g/L，Na2MoO4·2H2O 35～45g/L，AgNO38～10g/L；
2) Adjusting the pH value to 8.8-9.2 by using ammonia water, and adjusting the temperature to 65-75 ℃;
3) placing the inner crown with the surface soaked with silver into the prepared chemical plating solution for 10-15 min;
4) taking out the inner crown, air-drying in air for 5min, and washing with water.
2. A metal-ceramic coping, characterized by being produced by the production method according to claim 1.
CN201810726135.4A 2018-07-04 2018-07-04 Metal ceramic tooth inner crown and preparation method thereof Expired - Fee Related CN109044548B (en)

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