CN108403443A - A kind of dental cement and preparation method thereof - Google Patents
A kind of dental cement and preparation method thereof Download PDFInfo
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- CN108403443A CN108403443A CN201810163471.2A CN201810163471A CN108403443A CN 108403443 A CN108403443 A CN 108403443A CN 201810163471 A CN201810163471 A CN 201810163471A CN 108403443 A CN108403443 A CN 108403443A
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/831—Preparations for artificial teeth, for filling teeth or for capping teeth comprising non-metallic elements or compounds thereof, e.g. carbon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K6/00—Preparations for dentistry
- A61K6/80—Preparations for artificial teeth, for filling teeth or for capping teeth
- A61K6/884—Preparations for artificial teeth, for filling teeth or for capping teeth comprising natural or synthetic resins
- A61K6/891—Compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- Oral & Maxillofacial Surgery (AREA)
- Plastic & Reconstructive Surgery (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Dental Preparations (AREA)
Abstract
The present invention provides a kind of dental cements and preparation method thereof.Preparation method is as follows:(1)Methyl methacrylate is warming up to 100 110 DEG C, is slowly added to methyl acrylate, 2,4,6 trimethyl benzoyl diphenyl base phosphine oxides stir evenly, 20 40r/min of mixing speed, and mixing time is 180 300min;(2)50 65 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made fully to react;(3)After 30 60min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, lithium aluminosilicate, microcrystalline white mica powder, class sericite in powder are added while stirring, until stirring evenly;(4)After stirring, uniform irradiation 12h under gamma-rays, you can.The present invention dental cement adhesion strength by it is cold and hot influenced variation it is small, have smaller coefficient of thermal expansion.
Description
Technical field
The present invention relates to field of medical materials, and in particular to a kind of dental cement and preparation method thereof.
Background technology
In restoration of tooth, tissue of tooth is preserved as possible, protection dental pulp is one of cardinal principle.Minimal invasive dentistry is more
It is this principle have been pushed into forward major step, and the progress of Minimal invasive dentistry has benefited from vertex-gluing graph material and the hair of technology
Exhibition.As a kind of ideal binding material, it should stable physics and chemistry can be kept for a long time in oral environment complicated and changeable
Matter is not easily decomposed or dissolves, and is closely connect with tissue of tooth and dummy.It is also such as fiber post resin core dummy
This, the performance of resinoid bond directly influences the beauty and service life of dummy.Oral environment be it is extremely complex changeable,
Constantly there is salivary secretion, it is to cause to bond the major reason to fail to have body fluid circulatory, the environment of this high humility in dentine;Mouthful
Cavity temperature change greatly, binder is different from the coefficient of thermal expansion of tissue of tooth, this will be generated in temperature change thermal stress with
Micro blazed-grating causes repairing failure;Existing a large amount of bacteriums and its metabolite are easy to make binder that degradation aging occur in oral cavity,
Performance is caused to decline;In addition, the factors such as the stress of mastication processes generation and clinician's operation can all influence the effect of binder.
Invention content
Technical problems to be solved:The object of the present invention is to provide a kind of dental cements, overcome the shortcomings of above, bonding
Power is strong, and after cold cycling, adhesion strength variation is small.
Technical solution:A kind of dental cement is prepared by weight by following component:Methyl methacrylate 25-
35 parts, 40-60 parts of methyl acrylate, 0.3-2 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, nanometer hydroxyapatite
15-30 parts, 15-30 parts of silicon dioxide powder, 0.5-3 parts of organosilicon quaternary ammonium salt, 3-8 parts of lithium aluminosilicate, graphite flake/epoxy resin it is multiple
10-30 parts of condensation material, 10-20 parts of microcrystalline white mica powder, 10-20 parts of class sericite in powder, 30-60 parts of ethyl acetate.
It is further preferred that a kind of dental cement, is prepared by weight by following component:Metering system
Sour methyl esters 28-33 parts, 45-55 parts of methyl acrylate, 0.5-1.5 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, receive
18-23 parts of hydroxyapatite of rice, 18-23 parts of silicon dioxide powder, 1-2 parts of organosilicon quaternary ammonium salt, 4-7 parts of lithium aluminosilicate, graphite flake/
15-25 parts of epoxy resin composite material, 13-18 parts of microcrystalline white mica powder, 12-16 parts of class sericite in powder, ethyl acetate 45-55
Part.
The preparation method of above-mentioned dental cement, includes the following steps:
(1)Methyl methacrylate is warming up to 100-110 DEG C, is slowly added to methyl acrylate, 2,4,6- trimethylbenzoyls
Base diphenyl phosphine oxide stirs evenly, mixing speed 20-40r/min, mixing time 180-300min;
(2)It is cooled to 50-65 DEG C, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;
(3)After 30-60min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;
(4)After stirring, uniform irradiation 12h under gamma-rays, you can.
Further, the preparation method of a kind of dental cement, the step(1)In be warming up to 105 DEG C, stirring
Speed is 30r/min, mixing time 200-280min.
Further, the preparation method of a kind of dental cement, the step(2)In be cooled to 60 DEG C.
Further, the preparation method of a kind of dental cement, the step(3)The middle reaction time is 40min.
Further, the preparation method of a kind of dental cement, the step(3)Middle nanometer hydroxyapatite,
Silicon dioxide powder, microcrystalline white mica powder, class sericite in powder diameter 100-160nm.
Advantageous effect:The dental cement of the present invention is bonded in after cold cycling, and intensity decreased significantly, reason
It is that the coefficient of thermal expansion of common binding resin is higher than tissue of tooth, hot water can accelerate the hydrolysis of bonding interface ingredient, and constantly
The material interface that cold cycling can make the coefficient of expansion different generates stress, causes the generation in bonding interface gap, influences to bond strong
Degree.Microtensile bond strength retention rate is more than 90% after the cold cycling of embodiment, and the microtensile bond strength of comparative example retains
Rate is 70% or so.Embodiment microtensile bond strength retention rate is significantly larger than comparative example group, addition lithium aluminosilicate, graphite flake/
After epoxy resin composite material, microcrystalline white mica powder, class sericite in powder ingredient, the coefficient of thermal expansion of adhesive is reduced.
Specific implementation mode
Embodiment 1
A kind of dental cement is prepared by weight by following component:25 parts of methyl methacrylate, methyl acrylate 40
Part, 15 parts of silicon dioxide powder, has 0.3 part of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 30 parts of nanometer hydroxyapatite
3 parts of machine silicon quaternary ammonium salt, 3 parts of lithium aluminosilicate, 10 parts of graphite flake/epoxy resin composite material, 10 parts of microcrystalline white mica powder, class thin,tough silk cloud
20 parts of female powder, 30 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 100 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 20r/min, and mixing time is
180min;(2)50 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 60min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;(4)After stirring, uniform irradiation under gamma-rays
12h, you can.
Embodiment 2
A kind of dental cement is prepared by weight by following component:35 parts of methyl methacrylate, methyl acrylate 60
It is part, 2 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 15 parts of nanometer hydroxyapatite, 30 parts of silicon dioxide powder, organic
0.5 part of silicon quaternary ammonium salt, 8 parts of lithium aluminosilicate, 30 parts of graphite flake/epoxy resin composite material, 20 parts of microcrystalline white mica powder, class thin,tough silk cloud
10 parts of female powder, 60 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 110 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 40r/min, and mixing time is
300min;(2)65 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 30min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;(4)After stirring, uniform irradiation under gamma-rays
12h, you can.
Embodiment 3
A kind of dental cement is prepared by weight by following component:28 parts of methyl methacrylate, methyl acrylate 45
Part, 23 parts of silicon dioxide powder, has 0.5 part of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 18 parts of nanometer hydroxyapatite
2 parts of machine silicon quaternary ammonium salt, 4 parts of lithium aluminosilicate, 25 parts of graphite flake/epoxy resin composite material, 13 parts of microcrystalline white mica powder, class thin,tough silk cloud
16 parts of female powder, 45 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 105 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 30r/min, and mixing time is
200min;(2)60 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 40min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;(4)After stirring, uniform irradiation under gamma-rays
12h, you can.
Embodiment 4
A kind of dental cement is prepared by weight by following component:33 parts of methyl methacrylate, methyl acrylate 55
Part, 23 parts of silicon dioxide powder, has 1.5 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 18 parts of nanometer hydroxyapatite
1 part of machine silicon quaternary ammonium salt, 7 parts of lithium aluminosilicate, 15 parts of graphite flake/epoxy resin composite material, 18 parts of microcrystalline white mica powder, class thin,tough silk cloud
12 parts of female powder, 55 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 105 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 30r/min, and mixing time is
280min;(2)60 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 40min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;(4)After stirring, uniform irradiation under gamma-rays
12h, you can.
Embodiment 5
A kind of dental cement is prepared by weight by following component:30 parts of methyl methacrylate, methyl acrylate 50
It is part, 1 part of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 20 parts of nanometer hydroxyapatite, 22 parts of silicon dioxide powder, organic
1.5 parts of silicon quaternary ammonium salt, 6 parts of lithium aluminosilicate, 20 parts of graphite flake/epoxy resin composite material, 15 parts of microcrystalline white mica powder, class thin,tough silk cloud
14 parts of female powder, 50 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 105 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 30r/min, and mixing time is
240min;(2)60 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 40min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;(4)After stirring, uniform irradiation under gamma-rays
12h, you can.
Comparative example 1
A kind of dental cement is prepared by weight by following component:25 parts of methyl methacrylate, methyl acrylate 40
Part, 15 parts of silicon dioxide powder, has 0.3 part of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 30 parts of nanometer hydroxyapatite
3 parts of machine silicon quaternary ammonium salt, 10 parts of microcrystalline white mica powder, 20 parts of class sericite in powder, 30 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 100 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 20r/min, and mixing time is
180min;(2)50 DEG C are cooled to, ethyl acetate is sequentially added and continues to stir, it is made fully to react;(3)After 60min, while stirring
It mixes side and nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, microcrystalline white mica powder, class sericite in powder is added, until stirring
Uniformly;(4)After stirring, uniform irradiation 12h under gamma-rays, you can.
Comparative example 2
A kind of dental cement is prepared by weight by following component:35 parts of methyl methacrylate, methyl acrylate 60
It is part, 2 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, 15 parts of nanometer hydroxyapatite, 30 parts of silicon dioxide powder, organic
0.5 part of silicon quaternary ammonium salt, 8 parts of lithium aluminosilicate, 30 parts of graphite flake/epoxy resin composite material, 60 parts of ethyl acetate.
The preparation method of above-mentioned dental cement is:(1)Methyl methacrylate is warming up to 110 DEG C, is slowly added to third
E pioic acid methyl ester, 2,4,6-trimethylbenzoyldiphenylphosphine oxide stir evenly, mixing speed 40r/min, and mixing time is
300min;(2)65 DEG C are cooled to, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;(3)After 30min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, until stirring evenly;(4)After stirring, uniform irradiation 12h under gamma-rays, you can.
The adhesion strength of binder is unable to measure in oral cavity, generally all measures binder by experiment in vitro
Adhesion strength.This test method is to survey its power again within 24 hours in being bathed using the artificial saliva that will be soaked in 37 DEG C after bracket
Size, to obtain the result more close to oral cavity true environment.
Microtensile bond strength is tested:By each group tooth bonding testing piece under flowing water cooling, non-is pressed with cutting machine at a slow speed
Trimming technologies cut out the micro-stretching test specimen 5 of 1.0mm × 1.0mm × 6mm.502 glue are bonded in universal testing machine
It on fixture, is stretched under the loading velocity of 1mm/min, tests maximum load when its fracture, micrometer is used in combination accurately to measure
The bond area of each test specimen.
Adhesion strength calculation formula:Microtensile bond strength(MPa)=load(N)/ bond area(mm²).
ISO TR11405 regulations, cold cycling accelerated ageing should be recycled including at least 5 DEG C of 500 times and 55 DEG C of water-baths.It follows
The basic process of ring is residence time each 30s, passing time 20s, one cycle used time 100s in 5 DEG C and 55 DEG C of water-baths.This
Microtensile bond strength is tested after recycling 5000 times after experiment cold cycling.
If the adhesion strength of binder is more than 13.5Mpa, the damage of enamel can be caused when bracket falls off.The present invention
The property indices of material see the table below, it may be seen that this dental cement is bonded in after cold cycling, intensity is equal
It decreased significantly, the reason is that the coefficient of thermal expansion of common binding resin is higher than tissue of tooth, hot water can accelerate bonding interface ingredient
Hydrolysis, and constantly cold cycling can make the different material interface of the coefficient of expansion generate stress, cause bonding interface gap
It generates, influences adhesion strength.Microtensile bond strength retention rate is more than 90% after the cold cycling of embodiment, and comparative example is micro-
Tensile bond strength retention rate is 70% or so.Embodiment microtensile bond strength retention rate is significantly larger than comparative example group, is adding
After lithium aluminosilicate, graphite flake/epoxy resin composite material, microcrystalline white mica powder, class sericite in powder ingredient, adhesive is reduced
Coefficient of thermal expansion.
The microtensile bond strength of 1 dental cement of table compares
Name of product | Microtensile bond strength(MPa) | Microtensile bond strength after cold cycling(MPa) |
Embodiment 1 | 11.3 | 10.2 |
Embodiment 2 | 11.5 | 10.4 |
Embodiment 3 | 11.6 | 10.5 |
Embodiment 4 | 11.8 | 10.6 |
Embodiment 5 | 12.4 | 11.3 |
Comparative example 1 | 9.4 | 7.1 |
Comparative example 2 | 9.9 | 7.8 |
Claims (7)
1. kind of dental cement, which is characterized in that be prepared by weight by following component:Methyl methacrylate 25-35
Part, 40-60 parts of methyl acrylate, 0.3-2 parts of 2,4,6-trimethylbenzoyldiphenylphosphine oxide, nanometer hydroxyapatite
15-30 parts, 15-30 parts of silicon dioxide powder, 0.5-3 parts of organosilicon quaternary ammonium salt, 3-8 parts of lithium aluminosilicate, graphite flake/epoxy resin it is multiple
10-30 parts of condensation material, 10-20 parts of microcrystalline white mica powder, 10-20 parts of class sericite in powder, 30-60 parts of ethyl acetate.
2. a kind of dental cement according to claim 1, which is characterized in that prepared by weight by following component and
At:28-33 parts of methyl methacrylate, 45-55 parts of methyl acrylate, 2,4,6-trimethylbenzoyldiphenylphosphine oxide
0.5-1.5 parts, 18-23 parts of nanometer hydroxyapatite, 18-23 parts of silicon dioxide powder, 1-2 parts of organosilicon quaternary ammonium salt, lithium aluminosilicate
4-7 parts, graphite flake/15-25 parts of epoxy resin composite material, 13-18 parts of microcrystalline white mica powder, 12-16 parts of class sericite in powder, second
45-55 parts of acetoacetic ester.
3. a kind of preparation method of dental cement, which is characterized in that include the following steps:
(1)Methyl methacrylate is warming up to 100-110 DEG C, is slowly added to methyl acrylate, 2,4,6- trimethylbenzoyls
Base diphenyl phosphine oxide stirs evenly, mixing speed 20-40r/min, mixing time 180-300min;
(2)It is cooled to 50-65 DEG C, sequentially adds ethyl acetate, graphite flake/epoxy resin composite material continues to stir, it is made to fill
Divide reaction;
(3)After 30-60min, nanometer hydroxyapatite, silicon dioxide powder, organosilicon quaternary ammonium salt, alumina silicate are added while stirring
Lithium, microcrystalline white mica powder, class sericite in powder, until stirring evenly;
(4)After stirring, uniform irradiation 12h under gamma-rays, you can.
4. a kind of preparation method of dental cement according to claim 3, it is characterised in that:The step(1)Middle liter
Temperature is to 105 DEG C, mixing speed 30r/min, mixing time 200-280min.
5. a kind of preparation method of dental cement according to claim 3, it is characterised in that:The step(2)Middle drop
Temperature is to 60 DEG C.
6. a kind of preparation method of dental cement according to claim 3, it is characterised in that:The step(3)In it is anti-
It is 40min between seasonable.
7. a kind of preparation method of dental cement according to claim 3, it is characterised in that:The step(3)In receive
Rice hydroxyapatite, silicon dioxide powder, microcrystalline white mica powder, class sericite in powder diameter 100-160nm.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110693726A (en) * | 2019-11-07 | 2020-01-17 | 慧生医学科技(徐州)有限公司 | Dental caries repair material and preparation method thereof |
Citations (5)
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CN1146332A (en) * | 1996-08-26 | 1997-04-02 | 华西医科大学 | Non-mixing type oral cavity binder |
CN1252138A (en) * | 1997-04-11 | 2000-05-03 | 美国3M公司 | Ternary photoinitiator system for curing of epoxy resins |
CN1252137A (en) * | 1997-04-11 | 2000-05-03 | 美国3M公司 | Ternary photoinitiator system for curing of epoxy/polyol resin compositions |
CN101052679A (en) * | 2004-09-10 | 2007-10-10 | 汉斯化学股份公司 | Poly resin composition |
CN104873403A (en) * | 2015-05-21 | 2015-09-02 | 苏州市贝克生物科技有限公司 | Orthodontic adhesive and preparation method thereof |
-
2018
- 2018-02-27 CN CN201810163471.2A patent/CN108403443A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1146332A (en) * | 1996-08-26 | 1997-04-02 | 华西医科大学 | Non-mixing type oral cavity binder |
CN1252138A (en) * | 1997-04-11 | 2000-05-03 | 美国3M公司 | Ternary photoinitiator system for curing of epoxy resins |
CN1252137A (en) * | 1997-04-11 | 2000-05-03 | 美国3M公司 | Ternary photoinitiator system for curing of epoxy/polyol resin compositions |
CN101052679A (en) * | 2004-09-10 | 2007-10-10 | 汉斯化学股份公司 | Poly resin composition |
CN104873403A (en) * | 2015-05-21 | 2015-09-02 | 苏州市贝克生物科技有限公司 | Orthodontic adhesive and preparation method thereof |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110693726A (en) * | 2019-11-07 | 2020-01-17 | 慧生医学科技(徐州)有限公司 | Dental caries repair material and preparation method thereof |
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