CN1320873C - Resin base composite material dowel pin for dental surgery - Google Patents
Resin base composite material dowel pin for dental surgery Download PDFInfo
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- CN1320873C CN1320873C CNB2003101189671A CN200310118967A CN1320873C CN 1320873 C CN1320873 C CN 1320873C CN B2003101189671 A CNB2003101189671 A CN B2003101189671A CN 200310118967 A CN200310118967 A CN 200310118967A CN 1320873 C CN1320873 C CN 1320873C
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- dowel pin
- resin
- nanoparticle
- coupling agent
- long fiber
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Abstract
The present invention discloses a resin matrix composite material dowel pin and a preparation method thereof for dental surgeries. The composite material dowel pin uses resin matrix strengthened and toughened together by nanometer particles and long fiber processed by coupling agent solution. The preparation method of the composite material dowel pin comprises the steps: 1) using coupling agents to prepare acetone solution or alcohol solution, and adding nanometer particles into the acetone solution or the alcohol solution for the treatment of ultrasonic dispersion; 2) adding the nanometer particles processed by the coupling agent solution into the resin matrix; 3) using the long fiber as reinforcing material to ensure that the resin matrix fully infiltrates the long fiber; 4) lining the long fiber infiltrated fully by the resin along the dowel pin axially, and pressing the long fiber into shapes on a molding press by a technical requirement; and processing the long fiber into desired shapes and lengths according to clinical requirements after the long fiber is solidified, cooled and demoulded. The composite material dowel pin manufactured by the technical method greatly enhances toughness besides meeting the requirements for modulus and strength.
Description
Technical field
The present invention relates to a kind of tooth section with polymer matrix composites dowel pin and preparation method thereof, particularly long fibre and nanoparticle strengthen jointly, toughened resin based composites dowel pin and preparation method thereof.
Background technology
Known is the clinical method commonly used of tooth section with dowel pin making dowel crown reparation undesirable root, residual crown.Clinical widely used metal dowel pin is mainly considered from its intensity, maintenance aspect at present.Discover that behind metal dowel pin reparation pulpless tooth, there is the danger that causes the root folding much larger than tissue of tooth in the elastic modelling quantity of metal dowel pin; Simultaneously, the perishable variable color of metal dowel pin, light tight and influence attractive in appearance; Some element also might cause the danger of human allergy and chronic poisoning in the metal; In the clinical examination of tooth section, also can influence nuclear magnetic resonance etc.
The carbon fibre composite dowel pin has appearred abroad in twentieth century nineties, and is attractive in appearance because of its inherent black influence although its mechanical performance is more satisfactory, and its clinical practice is restricted.
The dowel pin combination property that glass fiber compound material is made is better, can satisfy the requirement of dentistry dowel pin in theory.The article " research of dental glass fiber reinforced composite resin " of document " practical stomatology magazine 1999 (15) 177 " Zhou Yongming, Shi Changxi, Chen Jihua, introduced employing E-glass fibre, acrylic resin prepares compound material dowel, bending strength and bending modulus meet the dowel pin requirement, but the toughness deficiency.
Summary of the invention
In order to overcome the insufficient shortcoming of prior art toughness, the invention provides a kind of tooth section with polymer matrix composites dowel pin and preparation method thereof.With the compound material dowel that the inventive method is made, its bending strength and modulus be near tooth essence, avirulence, and good biocompatibility, toughness improves.
The technical solution adopted for the present invention to solve the technical problems is: a kind of tooth section polymer matrix composites dowel pin, it is characterized in that: long fibre and the nanoparticle that employing was handled through coupling agent solution strengthens jointly, the toughened resin matrix, long stapled volume content is 55～65%, the nanoparticle weight content is 1～3% of a resin matrix, the volume content of resin matrix is 45～35%, and the coupling agent weight consumption is 0.8～1.5% of long fibre and a nanoparticle consumption.
Described long fibre is a glass fibre, high-strength glass fibre, and aramid fiber, or glass fibre, high-strength glass fibre and aramid fiber mix use.
Described nanoparticle is SiO
2, Al
2O
3, TiO
2, organo montmorillonite and meerschaum.
Described resin matrix adopts epoxy resin, epoxy acrylic resin and acrylic resin.
Described coupling agent should be selected silane coupler, titanate coupling agent for use according to different fiber types.
A kind of above-mentioned tooth section is characterized in that with the preparation method of polymer matrix composites dowel pin:
1) at first gets the coupling agent of nanoparticle consumption 0.8～1.5%, be mixed with acetone soln or alcoholic solution is stand-by, nanoparticle is put in acetone soln or the alcoholic solution, carry out ultrasonic dispersing and handled 15～20 minutes;
2) will join through the nanoparticle that coupling agent solution was handled in the resin matrix again, disperseed 15～20 minutes under 50～70 ℃ of temperature with the high speed homogenization dispersion machine, be warming up to 80～90 ℃, stirred 0.5～1 hour, make nanoparticle fully be distributed in the resin matrix;
3) will prepare resin adhesive liquid and pour in the glue groove, and make resin fully soak into long fibre;
4) long fibre that resin was fully soaked into is along the dowel pin axial arranging, adopt winding process, pultrude process, mould pressing process and resin transfer molding (RTM) process compression moulding on moulding press, curing, condition of cure is: solidified 0.8～1.2 hour at 80～100 ℃, being warmed up to 110～130 ℃ again solidified 0.8～1.2 hour, being warmed up to 140～150 ℃ solidified 1.8～2.4 hours, being warmed up to 170～190 ℃ solidified 1.8～2.4 hours, the back is cooled to room temperature with furnace temperature, is processed into required shape and length by clinical requirement after the demoulding.
The present invention's advantage compared to existing technology is, owing to adopt long fibre and nanoparticle strengthens jointly, the toughened resin matrix.The compound material dowel bending strength of made and modulus can prevent root folding and dowel pin brittle failure after implantation effectively near tooth essence; Adopt moulding processs such as winding, pultrusion and resin transfer moulding technology, the automaticity height, constant product quality, cost is low; This compound material dowel, not only bending strength and modulus be near tooth essence, and can be prepared near Dentinal color, and clinical practice is elegant in appearance.
The specific embodiment
Adopt long fibre and nanoparticle strengthens jointly, the toughened resin matrix.Nanoparticle is by after the coupling processing, adopt the high speed homogenization dispersion machine, under 20000 rev/mins and high shear force and high centrifugal force effect, nanoparticle fully is distributed in the resin matrix, nano particle diameter is little, specific surface area is big, a large amount of not molecule, the atoms of bonding are contained in the surface, have very high activity, can participate in the curing of resin matrix, the system crosslink density is increased, nano particle diameter is little simultaneously, by high speed dispersion, in the particle-filled free volume in polymer, further increased the modulus and the thermostability of system.Nanoparticle is well-dispersed in the resin matrix, because specific surface area is big, has a large amount of interfaces, after suffering reaction, can absorb a large amount of impact energys, and the toughness of system is increased, thereby has increased the toughness of compound material dowel.
Long fibre is given enough bending strengths of dowel pin and bending modulus along the dowel pin axial arranging, and fiber can adopt surperficial coupling agent treatment, and interfacial adhesion strength is improved.
The dowel pin preparation can be adopted winding process, pultrude process, mould pressing process, resin transfer molding (RTM) process, and curing process adopts traditional thermal curing methods, process for photocuring etc., obtains higher crosslink density with guarantee system.
Long fibre adopts glass fibre, as: E-GF, S-GF; Aramid fiber, as: Kevlar-49 etc.The volume content of fiber is 55～65%, and fiber is all along the axial unidirectional array of dowel pin, and for guaranteeing that bonding interface is good, fiber will adopt coupling agent treatment before use, thereby makes dowel pin have high mechanical property.
Nanoparticle can adopt SiO
2, Al
2O
3, TiO
2, organo montmorillonite, organise and handle meerschaum etc., addition is 1～3% of an amount of resin.
Coupling agent can adopt corresponding type according to different long fibres, and as silane coupler, titanate coupling agent etc., consumption is mixed with acetone soln or alcoholic solution and uses for handling 1% of material.
Resin matrix can adopt bisphenol A type epoxy resin, epoxy acrylic resin and acrylic resin.Curing mode is heat cure or photocuring.
Concrete preparation method is as follows:
(1) gets 1% coupling agent of nanoparticle consumption, be mixed with acetone soln or alcoholic solution.With the 1.5g nanoparticle, throw in 80～100ml, in 1% the coupling agent solution, adopt ultrasonic dispersing to handle 15～20 minutes.
(2) will join through the nanoparticle that coupling agent solution was handled in the 100g epoxy resin again, be warming up to 80 ℃, and adopt the high speed homogenization dispersion machine to disperse 15～20 minutes.
(3) will contain the 100g epoxy resin and the 50ml acetone uniform mixing of nanoparticle, and, as reinforcing material, adopt and twine legal system and be equipped with prepreg, hang cutting with S-GF as glue.
(4) with long fibre along the dowel pin axial arranging, adopt winding process, pultrude process, mould pressing process and resin transfer molding (RTM) process compression moulding on moulding press, curing, condition of cure is: 90 ℃/lh+120 ℃/lh+150 ℃/2h+180 ℃/2h.Furnace cooling gets the nano composite material dowel pin.
Application Example l:
Get 20 gram nanoparticle SiO
2, with 0.2 gram silane coupler KH-590, use the 100ml acetone diluted, regulating pH value is 7～9, fully disperseed 30 minutes with ultrasound wave, oven dry, stand-by.
Restrain the nanometer SiO that handled with 3
2, add in the 100 gram epoxy resin, be warming up to 50 ℃, stir the back slightly and disperseed 10 minutes, in boiling water bath, stir 1h again, about 60 ℃, add methyl tetrahydro phthalic anhydride then earlier with the high speed homogenization dispersion machine, add 1 gram 2-methyl again, the 4-ethyl imidazol(e) stirs gently, with the S-glass fibre as reinforcing material, adopt and squeeze drawing process, with mould and die preheating to 180 ℃, the glue for preparing is poured in the glue groove, make resin fully soak into fiber.Adjust hauling speed and traction apparatus jaw pressure, going out diameter at the 2cm/min compacted under is the cylindrical section bar of 1.4mm.Cut into Len req, be finished product.
Application Example 2:
Sepiolite in water, is removed impurity through dispersed with stirring, handles with dilute hydrochloric acid, filter, and washing, oven dry is pulverized.Join in the acetone at following surface treated 2 gram meerschaums of stirring, used ultrasonic Treatment then 30 minutes.Under stirring, with above-mentioned solution and 100 gram epoxy resin mix homogeneously, deviate from solvent, be warming up to 130 ℃, reacted l hour, on the high speed homogenization dispersion machine, disperseed 20 minutes again.The cooling back adds 70 gram methyl tetrahydro phthalic anhydrides, l gram 2-methyl, and the 4-ethyl imidazol(e), mix homogeneously, being mixed with proportion is 1.2g/cm
3Acetone soln.Adopt the s-glass fibre, the preparation prepreg, cold is at room temperature put, and makes volatile content less than 2%.Prepreg is cut into die size, and the shop overlays on and scribbles in the good steel mold of releasing agent and preheating, and through temperature programming, solidification temperature is 90 ℃/1h+120 ℃/1h+150 ℃/2h+180 ℃/2h, and behind the completion of cure, cooling and demolding promptly gets required dowel pin.
Claims (6)
1, a kind of tooth section polymer matrix composites dowel pin, it is characterized in that: long fibre and the nanoparticle that employing was handled through coupling agent solution strengthens jointly, the toughened resin matrix, long stapled volume content is 55～65%, the nanoparticle weight content is 1～3% of a resin matrix, the volume content of resin matrix is 45～35%, and the coupling agent weight consumption is 0.8～1.5% of long fibre and a nanoparticle consumption.
2, tooth according to claim 1 section polymer matrix composites dowel pin, it is characterized in that: described long fibre is a glass fibre, high-strength glass fibre, aramid fiber, or glass fibre, high-strength glass fibre and aramid fiber mix and use.
3, tooth according to claim 1 section polymer matrix composites dowel pin, it is characterized in that: described nanoparticle is SiO
2, Al
2O
3, TiO
2, organo montmorillonite and meerschaum.
4, tooth according to claim 1 section polymer matrix composites dowel pin, it is characterized in that: described resin matrix adopts epoxy resin, epoxy acrylic resin and acrylic resin.
5, tooth according to claim 1 section polymer matrix composites dowel pin is characterized in that: described coupling agent, should select silane coupler, titanate coupling agent for use according to different fiber types.
6, a kind of tooth as claimed in claim 1 section is characterized in that with the preparation method of polymer matrix composites dowel pin:
1) at first gets the coupling agent of nanoparticle consumption 0.8～1.5%, be mixed with acetone soln or alcoholic solution is stand-by, nanoparticle is put in acetone soln or the alcoholic solution, carry out ultrasonic dispersing and handled 15～20 minutes;
2) will join through the nanoparticle that coupling agent solution was handled in the resin matrix again, disperseed 15～20 minutes under 50～70 ℃ of temperature with the high speed homogenization dispersion machine, be warming up to 80～90 ℃, stirred 0.5～1 hour, make nanoparticle fully be distributed in the resin matrix;
3) will prepare resin adhesive liquid and pour in the glue groove, and make resin fully soak into long fibre:
4) long fibre that resin was fully soaked into is along the dowel pin axial arranging, adopt winding process, pultrude process, mould pressing process and resin transfer molding (RTM) process compression moulding on moulding press, curing, condition of cure is: solidified 0.8～1.2 hour at 80～100 ℃, being warmed up to 110～130 ℃ again solidified 0.8～1.2 hour, being warmed up to 140～150 ℃ solidified 1.8～2.4 hours, being warmed up to 170～190 ℃ solidified 1.8～2.4 hours, the back is cooled to room temperature with furnace temperature, is processed into required shape and length by clinical requirement after the demoulding.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101189671A CN1320873C (en) | 2003-12-09 | 2003-12-09 | Resin base composite material dowel pin for dental surgery |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2003101189671A CN1320873C (en) | 2003-12-09 | 2003-12-09 | Resin base composite material dowel pin for dental surgery |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1545986A CN1545986A (en) | 2004-11-17 |
| CN1320873C true CN1320873C (en) | 2007-06-13 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2003101189671A Expired - Fee Related CN1320873C (en) | 2003-12-09 | 2003-12-09 | Resin base composite material dowel pin for dental surgery |
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|---|---|
| CN (1) | CN1320873C (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104173196B (en) * | 2013-05-28 | 2018-01-12 | 南方医科大学南方医院 | Dental denture base fibre reinforced composites and preparation method thereof |
| CN104905981A (en) * | 2015-05-29 | 2015-09-16 | 苏州博利迈新材料科技有限公司 | Composite resin used for dental filling and preparation method thereof |
| CN112472610A (en) * | 2020-12-18 | 2021-03-12 | 内蒙古大学 | High SiO2Preparation method of pre-crown by adding amount of epoxy resin |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5964592A (en) * | 1997-07-21 | 1999-10-12 | Hites; Andras A. | Nonmetallic dental post and method |
| US6186791B1 (en) * | 1998-08-11 | 2001-02-13 | Jeneric/Pentron Incorporated | Fiber reinforced composite post |
-
2003
- 2003-12-09 CN CNB2003101189671A patent/CN1320873C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5964592A (en) * | 1997-07-21 | 1999-10-12 | Hites; Andras A. | Nonmetallic dental post and method |
| US6186791B1 (en) * | 1998-08-11 | 2001-02-13 | Jeneric/Pentron Incorporated | Fiber reinforced composite post |
Non-Patent Citations (4)
| Title |
|---|
| 偶联剂在环氧树脂/纳米SiO2复合材料中的应用 刘竞超，李小兵，杨亚辉，傅万里，张华林，中国塑料，第14卷第9期 2000 * |
| 齿科桩钉用纤维/树脂复合材料细胞毒性实验研究 张文云，施长溪，陈吉华，贾安琦，李南，中国美容医学，第11卷第4期 2002 * |
| 齿科聚合物基纤维纳米复合材料的力学性能研究 张文云，施长溪，陈吉华，赵信义，贾安琦，现代口腔医学杂志，第16卷第4期 2002 * |
| 齿科聚合物基纤维纳米复合材料的力学性能研究 张文云，施长溪，陈吉华，赵信义，贾安琦，现代口腔医学杂志，第16卷第4期 2002;齿科桩钉用纤维/树脂复合材料细胞毒性实验研究 张文云，施长溪，陈吉华，贾安琦，李南，中国美容医学，第11卷第4期 2002;偶联剂在环氧树脂/纳米SiO2复合材料中的应用 刘竞超，李小兵，杨亚辉，傅万里，张华林，中国塑料，第14卷第9期 2000 * |
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|---|---|
| CN1545986A (en) | 2004-11-17 |
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