CN109044548A - Hat and preparation method in a kind of metal-porcelain - Google Patents

Hat and preparation method in a kind of metal-porcelain Download PDF

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Publication number
CN109044548A
CN109044548A CN201810726135.4A CN201810726135A CN109044548A CN 109044548 A CN109044548 A CN 109044548A CN 201810726135 A CN201810726135 A CN 201810726135A CN 109044548 A CN109044548 A CN 109044548A
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hat
metal
porcelain
prepared
chemical plating
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CN109044548B (en
Inventor
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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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00Dental prostheses; Making same
    • A61C13/08Artificial teeth; Making same
    • A61C13/083Porcelain or ceramic teeth
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00Dental prostheses; Making same
    • A61C13/0003Making bridge-work, inlays, implants or the like
    • A61C13/0006Production methods
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/31Coating with metals
    • C23C18/42Coating with noble metals
    • C23C18/44Coating with noble metals using reducing agents
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C18/00Chemical 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
    • C23C18/16Chemical 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
    • C23C18/48Coating with alloys
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C28/00Coating 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
    • C23C28/02Coating 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
    • C23C28/021Coating 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61CDENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C2201/00Material 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)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • 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 present invention provides hat and preparation methods in a kind of metal-porcelain, and surface will be preced in metal-porcelain and first carries out leaching silver, carries out chemical plating Fe-Ag-Mo-B again after soaking silver processing.Hat reduces the activity of metal by leaching silver processing in metal tooth, is conducive to surface and carries out chemical plating;The surface stress being preced in metal is reduced after chemical plating Fe-Mo-Ag-B, and the B element good with Ceramic bond is contained on surface layer, keep hat in metal tooth good with dental polishing associativity during the porcelain in later period, increase Metal-ceramic combining strength, Fe, Mo element can enhance the biocompatibility being preced in tooth, and Ag element assigns antibacterial functions.

Description

Hat and preparation method in a kind of metal-porcelain
Technical field
The invention belongs to Metal-porcelain technical field, in particular to hat and preparation method in a kind of metal-porcelain.
Background technique
According to statistics, China has nearly 900,000,000 people with gingivitis and periodontitis.As horizontal the stepping up of people is controlled with patient Treat the enhancing of consciousness, dental clinic and scientific research rapidly develop, metal-porcelain using more and more extensive.Metal-porcelain be through High temperature, which melts porcelain powders, is attached to the mouth mending material formed on composite material ground, and baking-ceramic tooth is exactly that coating is labeled in metal tooth One layer of glaze class material melts frit material to form the dummy of the color for being similar to dermal tooth and gloss by high-temperature calcination, Have the characteristics that intensity height, good toughness, corrosion resistance be strong and preferable biocompatibility.
Crown root mainly includes billon, stainless steel, nickel chromium triangle according to the different classifications used with preparation process in metal-porcelain Alloy, cochrome etc..Billon is expensive, remaining several alloy contains nickel, chromium, cobalt etc. in varying degrees and is harmful to the human body Element, be easy to make that allergy occurs for patient and black line phenomenon occurs in gum, so stainless steel, nichrome, cochrome etc. are roasting Hat is gradually withdrawn from the market in porcelain tooth.Compared to these materials, it is lower, resistance to that titanium alloy material has specific strength height, elasticity modulus The advantages that corrosivity, therefore gradually by extensive concern and research.But titanium alloy exists such as the interior hat of metal-porcelain Lower deficiency: 1. golden porcelain combines poor, is easy to appear and collapses porcelain phenomenon;2. the bacteria's numbers and species in oral cavity are many and diverse, titanium alloy is commonly used There is no antibacterial action;3. poor biocompatibility.
Domestic number of patent application is 201610967676.7 to provide hat and its preparation side in a kind of metal ceramics dummy Method is preced with plating TiN film by way of sputtering in titanium alloy, and it is exposed and improve the gold of later period porcelain process to avoid metallochrome Porcelain bond strength, but without solving antibiotic property and biocompatibility issues.
Summary of the invention
To solve the above-mentioned problems, it the present invention provides hat and preparation method in metal-porcelain, can solve the problems, such as follows: 1. improving the Metal-ceramic combining strength of hat and dental polishing in tooth;2. having certain antibacterial effect;3. good biocompatibility.
Based on object above, the present invention provides hat and preparation methods in a kind of metal-porcelain, it is characterised in that: in tooth Hat surface first carries out leaching silver, carries out chemical plating Fe-Ag-Mo-B again after soaking silver processing.
Hat and preparation method, preparation process in roasting metal-porcelain provided by the invention are as follows:
(1) leaching silver processing, comprising the following steps:
1) immersion plating liquid: 15~20g/L of silver nitrate, 205~225g/L of thiocarbamide is prepared;
2) it is 3.9~4.2 with hydrochloric acid adjustment pH value, guarantees 20~30 DEG C of temperature;
3) it is prepared in titanium alloy and is preced with according to tooth mould, interior hat is put into dehydrated alcohol ultrasonic cleaning 5min, uses deionized water It is dried up after cleaning;
4) interior hat is put into 1.5~2.2min of holding in prepared immersion plating liquid;
5) interior hat is taken out, is washed after hanging 5min in air.
(2) chemical plating Fe-Ag-Mo-B, comprising the following steps:
1) chemical plating fluid: FeSO is prepared4·7H2O 18~22g/L, KNaC4H4O6·4H2O 85~95g/L, KBH45~ 10g/L, NaOH 16~24g/L, Na2MoO4·2H2O 35~45g/L, AgNO38~10g/L;
2) with ammonium hydroxide adjustment pH value be 8.8~9.2,65~75 DEG C of temperature;
3) the interior hat of surface leaching silver is put into 10~15min of holding in prepared chemical plating fluid;
4) interior hat is taken out, is washed after hanging 5min in air.
Hat is reduced the activity being preced in metal tooth, is conducive to by leaching silver processing in metal-porcelain provided by the present invention Surface carries out chemical plating.
Hat reduces hat in metal tooth by surface chemical plating Fe-Mo-Ag-B in metal-porcelain provided by the present invention Surface stress, and the B element good with Ceramic bond is contained on surface layer, and hat in tooth is made to make pottery during the porcelain in later period with dentistry Conjunction property is good by force for porcelain, increases Metal-ceramic combining strength, and Fe, Mo element can enhance the biocompatibility being preced in tooth, and Ag element assigns anti- Bacterium function.
The present invention has the advantage that and is 1. subtracted by chemical plating Fe-Ag-Mo-B compared with being preced in existing titanium alloy tooth The surface stress being preced in small titanium alloy, and B element is contained on surface layer, keeps the Metal-ceramic combining strength of interior hat and dental polishing high;② Reach antibacterial effect using the Ag element of addition;3. Fe, Mo element, good biocompatibility are contained in hat surface layer in metal-porcelain.
Specific embodiment
Principles and features of the present invention are described with reference to embodiments, listed give an actual example is served only for explaining this hair It is bright, not limit the scope of the invention.
Embodiment 1:
Hat and preparation method, include the following steps: in a kind of metal-porcelain
1) leaching silver: immersion plating liquid: silver nitrate 15g/L, thiocarbamide 210/L is 1. prepared;2. being 4.0 with hydrochloric acid adjustment pH value, guarantee 25 DEG C of temperature;It is preced with 3. being prepared in titanium alloy according to tooth mould, interior hat is put into dehydrated alcohol ultrasonic cleaning 5min, uses deionized water It is dried up after cleaning;4. interior hat is put into prepared immersion plating liquid and keeps 2.0min;5. interior hat is taken out, 5min is hung in air After wash.
2) chemical plating Fe-Ag-Mo-B: chemical plating fluid is 1. prepared: FeSO4·7H2O 19g, KNaC4H4O6·4H2O 92g, KBH48g, NaOH 20g, Na2MoO4·2H2O 40g, AgNO39g adds water to 1L;2. being 9.0 with ammonium hydroxide adjustment pH value, guarantee 65 DEG C of temperature;3. the interior hat of surface leaching silver is put into prepared chemical plating fluid and keeps 15min;4. interior hat is taken out, air In hang 5min after wash.
3) antibacterial experiment: hat in the metal-porcelain made being cleaned by ultrasonic through dehydrated alcohol, deionized water, each 8min, It is then placed in 75% alcoholic solution of volume fraction and sterilizes 45min.Test bacterium is staphylococcus aureus, porphyromonas unit cell Bacterium.It will be preced with and put into culture dish in the metal-porcelain after disinfection first, 50mL bacteria suspension, static gas wave refrigerator 2h, so that carefully is added Bacterium is sufficiently sticked.The bacterium that surface porosity is sticked is rinsed out with PBS solution later, is rinsed 3 times altogether.Metal after will be flushed Hat is put into 50mLPBS solution in baking-ceramic tooth, and sonic oscillation 3min rinses out the bacterium of surface adhesion.Table will be contained later The PBS solution of face adherent bacteria takes 5mL, is uniformly layered on plate, plate is put into 37 DEG C of constant incubator 12h is cultivated, observation calculates clump count.
4) it is thin that surfacing position inoculation neonate rat skull skeletonization biocompatibility experiment: is preced in metal-porcelain Born of the same parents, inoculum density are 300/mm2, with the DMEM culture medium culture for the newborn bovine serum for being 10% containing volume fraction, every 1d Liquid is changed, cultivates 3d and 5d respectively, then MTT 0.1mL, 37 DEG C of culture 4h are added in every hole, inhale and abandon supernatant, then every hole is added DMSO 0.5mL measures absorbance with microplate reader at wavelength 490nm.
Embodiment 2:
Hat and preparation method, include the following steps: in a kind of metal-porcelain
1) leaching silver: immersion plating liquid: silver nitrate 18g/L, thiocarbamide 212g/L is 1. prepared;2. being 4.2 with hydrochloric acid adjustment pH value, guarantee 25 DEG C of temperature;It is preced with 3. being prepared in titanium alloy according to tooth mould, interior hat is put into dehydrated alcohol ultrasonic cleaning 5min, uses deionized water It is dried up after cleaning;4. interior hat is put into prepared immersion plating liquid and keeps 2.2min;5. interior hat is taken out, 5min is hung in air After wash.
2) chemical plating Fe-Ag-Mo-B: chemical plating fluid is 1. prepared: FeSO4·7H2O 21g, KNaC4H4O6·4H2O 91g, KBH48.5g, NaOH 21g, Na2MoO4·2H2O 45g, AgNO310g adds water to 1L;2. it is 9.2 with ammonium hydroxide adjustment pH value, Guarantee temperature 70 C;3. the interior hat of surface leaching silver is put into prepared chemical plating fluid and keeps 12min;4. interior hat is taken out, It is washed after hanging 5min in air.
3) it antibacterial experiment: is carried out by embodiment 1.
4) it biocompatibility experiment: is carried out by embodiment 1.
Embodiment 3:
Hat and preparation method, include the following steps: in a kind of metal-porcelain
1) leaching silver: immersion plating liquid: silver nitrate 15g/L, thiocarbamide 205g/L is 1. prepared;2. being 3.9 with hydrochloric acid adjustment pH value, guarantee 20 DEG C of temperature;It is preced with 3. being prepared in titanium alloy according to tooth mould, interior hat is put into dehydrated alcohol ultrasonic cleaning 5min, uses deionized water It is dried up after cleaning;4. interior hat is put into prepared immersion plating liquid and keeps 1.5min;5. interior hat is taken out, 5min is hung in air After wash.
2) chemical plating Fe-Ag-Mo-B: chemical plating fluid is 1. prepared: FeSO4·7H2O 18g, KNaC4H4O6·4H2O 85g, KBH45~10g, NaOH 16g, Na2MoO4·2H2O 35g, AgNO38g adds water to 1L;2. it is 8.8 with ammonium hydroxide adjustment pH value, Guarantee 75 DEG C of temperature;3. the interior hat of surface leaching silver is put into prepared chemical plating fluid and keeps 10min;4. interior hat is taken out, It is washed after hanging 5min in air.
3) it antibacterial experiment: is carried out by embodiment 1.
4) it biocompatibility experiment: is carried out by embodiment 1.
Comparative example 1:
Hat and preparation method, include the following steps: in a kind of metal-porcelain
1) chemical plating Fe-Ag-Mo-B: chemical plating fluid is 1. prepared: FeSO4·7H2O 18g, KNaC4H4O6·4H2O 85g, KBH45~10g, NaOH 16g, Na2MoO4·2H2O 40g, AgNO39g adds water to 1L;2. it is 8.8 with ammonium hydroxide adjustment pH value, Guarantee 75 DEG C of temperature;3. the interior hat of surface leaching silver is put into prepared chemical plating fluid and keeps 10min;4. interior hat is taken out, It is washed after hanging 5min in air.
2) it antibacterial experiment: is carried out by embodiment 1.
3) it biocompatibility experiment: is carried out by embodiment 1.
Comparative example 2:
Hat and preparation method, include the following steps: in a kind of metal-porcelain
1) hat in titanium alloy is prepared.
2) it antibacterial experiment: is carried out by embodiment 1.
3) it biocompatibility experiment: is carried out by embodiment 1.
Embodiment and comparative example obtain that the results are shown in Table 1.
Table 1
Embodiment and comparative example shows in table 1: being 1. preced with after passing through leaching silver chemical plating Fe- again in Examples 1 to 3 in titanium alloy Ag-Mo-B reduces the surface stress being preced in titanium alloy, and the B element good with Ceramic bond is contained on surface layer, and hat in tooth is made to exist Conjunction property is good by force with dental polishing during the porcelain in later period, increases Metal-ceramic combining strength, and comparative example 1 is not soaked silver-colored but direct Chemical plating Fe-Ag-Mo-B, Metal-ceramic combining strength are then greatly reduced, and illustrate without soaking silver but direct electroless plating Fe-Ag-Mo-B Binding force is weak, and comparative example 2 is then that hat, Metal-ceramic combining strength are lower in general titanium alloy;2. except comparative example 2 does not have chemical plating Outside Fe-Ag-Mo-B, other 4 all have preferable antibacterial effect and biocompatibility, illustrate that Ag element imparts antibacterial function Can, Fe, Mo element can enhance the biocompatibility being preced in tooth.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.

Claims (3)

1. hat and preparation method in a kind of metal-porcelain, which is characterized in that hat surface first carries out leaching silver, leaching silver in titanium alloy tooth Chemical plating Fe-Ag-Mo-B is carried out after processing again.
2. hat and preparation method in metal-porcelain according to claim 1, which is characterized in that silver leaching process includes as follows Step:
1) immersion plating liquid: 15~20g/L of silver nitrate, 205~225g/L of thiocarbamide is prepared;
2) it is 3.9~4.2 with hydrochloric acid adjustment pH value, guarantees 20~30 DEG C of temperature;
3) it is prepared in titanium alloy and is preced with according to tooth mould, interior hat is put into dehydrated alcohol ultrasonic cleaning 5min, is cleaned with deionized water After dry up;
4) interior hat is put into 1.5~2.2min of holding in prepared immersion plating liquid;
5) interior hat is taken out, is washed after hanging 5min in air.
3. hat and preparation method in metal-porcelain according to claim 1, which is characterized in that chemical plating Fe-Ag-Mo-B Technique includes the following steps:
1) chemical plating fluid: FeSO is prepared4·7H2O 18~22g/L, KNaC4H4O6·4H2O 85~95g/L, KBH45~10g/ L, NaOH 16~24g/L, Na2MoO4·2H2O 35~45g/L, AgNO38~10g/L;
2) with ammonium hydroxide adjustment pH value be 8.8~9.2,65~75 DEG C of temperature;
3) the interior hat of surface leaching silver is put into 10~15min of holding in prepared chemical plating fluid;
4) interior hat is taken out, is washed after hanging 5min in air.
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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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114366361A (en) * 2022-01-04 2022-04-19 北京劲松口腔医院投资管理有限公司 Preparation process of porcelain tooth

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