WO2008041747A1

WO2008041747A1 - Member for dental purposes and process for production thereof

Info

Publication number: WO2008041747A1
Application number: PCT/JP2007/069477
Authority: WO
Inventors: Toshio Teranaka; Koji Hanaoka; Takahiro Tanaka; Masuji Yamaguchi; Toyohiko Shindo
Original assignee: Contamination Control Services
Priority date: 2006-10-04
Filing date: 2007-10-04
Publication date: 2008-04-10
Also published as: JP5154428B2; JPWO2008041747A1

Abstract

Disclosed is a member for dental purposes, which comprises a main body of the member and a silica film comprising polysilazane and formed on the main body, wherein the surface of the silica film is treated with a silane coupling agent. Also disclosed is a process for producing a member for dental purposes, which comprises the steps of: applying a coating solution comprising polysilazane onto a main body of the member and converting the polysilazane into silica, thereby forming a silica film; and treating the surface of the silica film with a silane coupling agent.

Description

Specification

Dental member and manufacturing method thereof

Technical field

The present invention relates to a dental member and a manufacturing method thereof.

This application (October 2006, April 4, 2006, No. 2006-272960, Japanese Patent Application No. 2006-272960 filed with priority, and the contents of which are incorporated herein by reference.

Background art

[0002] For example, resin cements or resin-added glass ionomer cements for bonding crown restorations such as crowns, inlays, and bridges to teeth and abutment tooth materials (metals, resins, ceramics, etc.) Dental adhesives are used.

Adhesion of dental parts such as crown restorations requires high adhesive strength, and various adhesion methods have been proposed for this purpose.

[0003] For example, in Patent Document 1 below, when a synthetic resin crown prosthesis is bonded to a glass ionomer cement, metatalylate or attalylate having an unsaturated double bond, an organic titanate compound, and a polymerization initiator are used. The following Patent Document 2 proposes a metatalylate-based polymerization as an adhesive when adhering a crown restoration material made of calcium phosphate-based crystallized glass to a tooth or an abutment tooth material. A method using an adhesive containing a sex monomer is described.

Patent Document 3 below contains an acidic group-containing radical polymerizable monomer, a non-acidic radical polymer monomer, a chemical polymerization initiator and a filler, and 2, 4 diphenyl 4-methyl- 1 A method using a dental adhesive containing pentene has been proposed. Patent Document 1: Japanese Patent Laid-Open No. 5-155728

Patent Document 2: JP-A-9 087124

Patent Document 3: Republished Patent WO2003 / 057180 Pamphlet

Disclosure of the invention

Problems to be solved by the invention [0004] However, since the methods described in Patent Documents 1 to 3 use a new adhesive, it is not easy to establish a method of use and formulation for practical use. In addition, sufficient adhesive strength may not be obtained, and particularly when the dental member is made of metal, the adhesive strength is insufficient.

[0005] The present invention has been made in view of the above circumstances, and an object of the present invention is to enable a dental member to be bonded with high adhesive strength.

Means for solving the problem

[0006] In order to solve the above problems, the dental member of the present invention is provided with a silica film generated from polysilazane on the dental member body, and the silica film is surface-treated with a silane coupling agent. Processed! /, Characterized in that.

The present invention also includes a step of applying a coating liquid containing polysilazane onto a dental member body, and then converting the polysilazane to silica to form a silica film; and the silica film is formed with a silane coupling agent. There is provided a method for producing a dental member characterized by having a surface treatment step.

[0007] In the method for producing a dental member, preferably, the silica film is subjected to surface treatment with the silane coupling agent after being irradiated with ultraviolet rays.

Further, instead of irradiating with ultraviolet rays, it is also preferable that the silica film is surface-treated with the silane coupling agent after being sprayed with flames or plasma in a water vapor atmosphere while spraying fine water droplets of water. Masle.

Further, the silica film may be subjected to a surface treatment with the silane coupling agent after spraying a minute water droplet of hydrogen peroxide water or in a vapor atmosphere of hydrogen peroxide water after flame irradiation or plasma irradiation. I like it.

The invention's effect

[0008] According to the present invention, the adhesive strength between the dental member and the adherend can be improved.

Brief Description of Drawings

FIG. 1 is a schematic configuration diagram showing a first example of a dental member of the present invention.

FIG. 2 is a schematic configuration diagram showing a second example of the dental member of the present invention.

FIG. 3 is a schematic configuration diagram showing a third example of the dental member of the present invention. FIG. 4 is a diagram showing an FT-IR spectrum of the silica film obtained in the example.

FIG. 5 is a schematic diagram for explaining an evaluation method of adhesive strength.

6] A schematic diagram of an apparatus for measuring adhesive strength.

Explanation of symbols

ι 、 ι 、、 11 Dental body

2, 2, 12 Silica membrane

3, 3, 13 Surface treatment layer with silane coupling agent

4, 4 ', 14 Dental parts

5 Adhesive

6, 15

21 Base material (test piece)

21a Adhesive surface

22 Adhesive tape

23 methanol rod

BEST MODE FOR CARRYING OUT THE INVENTION

[0011] Figs.! To 3 are schematic configuration diagrams showing first to third examples of the dental member of the present invention, but the present invention is not limited to these.

In the figure, reference numerals 1, 1 'and 11 denote dental member main bodies (hereinafter also abbreviated as main bodies), 2, 2' and 12 denote silica films, and 3, 3 'and 13 denote silane cups. A surface treatment layer with a ring agent (hereinafter sometimes referred to as a silane coupling layer) is shown, and 4, 4 'and 14 are dental members.

The dental member of the present invention may be one in which the dental member 4 is bonded to the adherend 6 via the adhesive 5 as in the example of FIG. For example, a prosthetic device (dental member 4) is attached to a tooth (bonded object 6) with an adhesive 5.

Alternatively, as in the example of FIG. 2, the dental members 4 and 4 ′ may be bonded to each other through the adhesive 5. For example, the prosthetic device (dental member 4) is attached to the abutment device (dental member 4 ') via the adhesive 5.

Alternatively, as in the example of FIG. 3, the dental member 14 and the adherend 15 made of a resin may be directly bonded. For example, a resin layer (adhesive 15) is provided on the dental member 14 to provide a prosthesis. This is a mode in which a device is manufactured or a mode in which a prosthetic device is manufactured by adhering another member (bonded object 15) having a resin force to the dental member 14.

[0013] Specific examples of the dental member body 1 in the examples of Figs. 1 and 2 include a metal inlay, a metal onlay, a metal crown, a metal bridge, a hard (composite) resin front crown, and a hard (composite) resin front dress. Metal dental technology such as bridges, porcelain baked iron crowns, porcelain baked iron bridges, Konus krone inner crowns, metal post cores, metal root plates, adhesive bridges, etc .; Ceramic dental technicians such as crowns, all ceramic bridges, laminate bearings, ceramic scores (ceramic cores); hard (composite) resin inlays, hard (composite) resin onlays, and hard (composite post cores) Dental technicians; orthodontic appliances such as brackets and bands; lip bumpers, rapid expansion equipment Straightening retainers such as a mandibular canine interdental retainer; fixed-type space retaining devices such as a dental shroud, crown loop, lingual arch; and magnetic attachments.

[0014] Specific examples of the adherend 6 in the example of Fig. 1 include a tooth (enamel, dentin), a metal core (metal abutment), a ceramic score (a porcelain core), a resin core, and the like.

In the example of Fig. 2, examples of the dental member body 1 'on the adherend side to be bonded to the dental member 4 include a metal core (metal abutment), a ceramic score (a porcelain core), and a resin core. .

[0015] In the examples of FIGS. 1 and 2, the materials of the dental member bodies 1 and 1 'are high carat gold alloy (Typel-4), platinum metal, multi-purpose gold alloy, low carat gold alloy, gold Palladium alloy, gold silver Palladium alloy, silver alloy, cobalt chromium alloy, nickel chromium alloy, titanium, titanium alloy, stainless steel (SUS304), magnetic stainless steel, and other general dental metals; alumina porcelain, castable Ceramics, pressure moldable porcelain, glass permeable ceramics, high density sintered (CAD / CAM) ceramics, high-purity alumina, ginolecoyu, partially stabilized zircoua, apatite ceramics, other general dental ceramics and Inorganic materials; composite resins, polycarbonates, and other general dental resins. In particular, the effect of the present invention is great when the dental member body 1, 1 'is made of metal or ceramics.

As the adhesive 5 in the examples of FIGS. 1 and 2, a resin adhesive commercially available as a dental adhesive / adhesive material can be used as appropriate. A resin cement or a resin-added glass ionomer cement is preferred in that the effect of improving the adhesive strength according to the present invention is more excellent.

Examples of resin cements that can be suitably used include Kuraray Medical's Panavia Fluoro Cement (product name), Tokumadental's Bistight II (product name), and GSI's Link Max (product name).

Examples of glass ionomer resin cements that can be suitably used include FUJI ROUTING S (product name) by GS, Fuji Luute (BC) (product name) by GS, and Vitremer routing cement (product by 3M ESPE) Name).

In FIG. 3, as a specific example of an embodiment in which a resin layer (adhered object 15) is provided on a dental member body 11 via a silica film 12 and a silane coupling layer 13, a metal crown or a metal bridge is used. Adhesion of metal frame and opaque resin in Cornus' telescope crown; Resin anterior of metal attachment denture device; Metal implant Superstructure (composite resin); Resin anterior on clasp Etc. In FIG. 3, as a specific example of an aspect in which a hard (composite) resin force is bonded to the dental member 14 via the silica film 12 and the silane coupling layer 13, another member (adhered material 15) is bonded. Adhesion of metal floor or metal framework to floor resin in artificial denture; Adhesion of resin floor denture to metal clasp, metal bar or metal framework; Adhesion of magnetic attachment to floor resin; Porcelain tooth and floor Adhesion with resin for use

Yes

In addition, the mode shown in Fig. 3 consists of jaw denture; epithesis device; speech function, speech lift, language lift recovery device such as nominal lift; floor correction device (occlusal slope plate, occlusal lift plate), enlargement device (rapid, slow), function Devices (activator, bionator, Frenkel device, Bimler's adapter), multi-bracket device, labial lingual arc device, etc .; removable restraint devices such as a horley type retainer and a wrap and retainer; And removable clearance It can be applied to adhesion between a metal member and a resin member in an apparatus or the like.

The material of the dental member body 11 in the example of FIG. 3 is the same as the material of the dental member bodies 1 and 1 ′ in the examples of FIGS.

Examples of the material of the adherend 15 include a composite resin, a denture base polymerization acrylic resin, a denture base thermoplastic resin, an artificial tooth acrylic resin, and other general dental resins.

The silica film 2 (2 ′, 12) in the examples of FIGS. 1 to 3 is a film generated from polysilazane. Specifically, the coating liquid containing polysilazane and a solvent is applied to the dental member body 1 (1 ′, 11), and then the solvent is removed and the polysilazane is converted into silica.

The silica film in the present invention means a film containing silica converted from a polysilazane film, and not all of the polysilazane is necessarily converted to silica.

The polysilazane used in the present invention is “one (SiH 2 —NH) one” (provided that all of H or all

2

A part may be substituted with a substituent. ) As a repeating unit, such as chain polysilazane and cyclic polysilazane.

Examples of the chain polysilazane include perhydropolysilazane, polymethylhydrosilazane, poly N-methylsilazane, poly N- (triethylsilyl) arylsilazane, poly N- (dimethylamino) cyclohexylsilazane, and phenylpolysilazane. All of these can be used and are not limited to these. In addition, polysilazane may be used alone or as a mixture of two or more.

Among the examples listed above, perhydroxypolysilazane is particularly preferable in that the effect of improving the adhesive strength according to the present invention is good.

[0020] The solvent contained in the coating liquid may be any solvent that does not react with polysilazane and can form a uniform polysilazane solution. Specific examples include aromatic hydrocarbons such as benzene, toluene, xylene, and ethylbenzene; aliphatic hydrocarbons such as pentane, hexane, isohexane, methyl pentane, heptane, isoheptane, octane, and isooctane; Cycloaliphatic hydrocarbons such as methylcyclopentane, cyclohexane, methylcyclohexane; methylene chloride, black-form, carbon tetrachloride, bromoform, ethylene chloride, Halogenated hydrocarbons such as chloroidylidene, trichloroethane, etc .; And ethers. These solvents may be one or a mixture of two or more! /.

The concentration of polysilazane in the coating solution is preferably 0.0;! -50 mass%, more preferably 1-20 mass%.

A catalyst may be added to the coating solution. Examples of the catalyst include amines such as triethylamine, dimethylamine, monoethanolamine, diethanolamine, n-butylamine, di-n-butylamine, and tri-n-butylamine, and metal hydroxides such as sodium hydroxide and potassium hydroxide. , Bases such as aqueous ammonia and pyridine, acetic acid, acetic anhydride, succinic acid, fumaric acid, maleic acid, maleic anhydride, carboxylic acids such as succinic acid and their anhydrides, organic acids such as trichloroacetic acid, hydrochloric acid, nitric acid And inorganic acids such as sulfuric acid, and Lewis acids such as iron trichloride and aluminum trichloride.

[0021] The dental member of the present invention can be produced, for example, by the following method.

First, the coating liquid is applied to the adhesive surface of the dental member body 1 (1 ′, 11). As a coating method, a brush coating method, a spray method, a dipping method, a flow coating method, or the like can be used. Prior to application of the coating solution, the adhesive surface of the main body 1 (1 ', 11) may be polished or washed as necessary.

It is preferable to perform a drying process to remove the solvent after applying the coating solution. After drying, polysilazane is converted to silica to form a silica film.

[0022] As a method of converting polysilazane to silica, a known method can be appropriately used. Examples include (1) a method of conversion by heating, (2) a method of conversion by ultraviolet irradiation, and (3) a method of conversion by exposure to ammonia water vapor.

(1) In the method by heating, for example, a coating liquid containing polysilazane is applied to a substrate, dried in the atmosphere for about 10 minutes, and then at room temperature to 900 ° C, preferably 90 to 600 ° C. It is converted into a silica film by heat treatment for 1 to 6 hours, preferably 0.5 to 4 hours. Conditions can be changed as appropriate (the same shall apply hereinafter).

Alternatively, as described in JP-A-8-27425, a coating containing polysilazane is used. After applying the coating liquid to the substrate, pre-cured at 150 ° C for 1 hour in an air atmosphere, and then converted to a silica film by heating at 95 ° C under atmospheric pressure for 3 hours in an 80% RH atmosphere. Use force S

(2) The method of ultraviolet irradiation is, for example, described in Journal of the Ceramic Society of Japan 112 [11] 599-603 (2004), and the coating liquid containing polysilazane is used as the base material. After coating, the film can be dried at 40 ° C for about 10 minutes, and then can be converted into a silica film by irradiation with 172 nm UV light for about 60 minutes in a 20% oxygen atmosphere.

(3) For example, Journal of Sol-Gel Scienc and Technology 31, 257-261 (2004). The method using ammonia water vapor exposure is based on a coating liquid containing polysilazane. After being applied to the film, it can be converted to a silica film by exposure to ammonia vapor of lmol / L for 24 hours.

In any of the above methods (1) to (3), polysilazane reacts with moisture in the atmosphere and is converted to silica to form a silica film.

[0023] (1) In the heating method, particularly when heated in a high humidity environment, a hydrophilic silica film having an OH group bonded to a silicon atom (Si) is produced. The relative humidity in the high humidity environment is preferably 50% RH or more. When the hydrophilic silica film is formed, the effect of improving the adhesion strength according to the present invention can be obtained better.

Alternatively, even if the portion to which the coating liquid is applied is treated with a hydrophilizing agent, a hydrophilic sili-fibrous film can be generated. As a method of treating with a hydrophilizing agent, a method of immersing the coating solution in a hydrophilizing agent after application and drying it after drying, a method of immersing the coating solution in a hydrophilizing agent after application, and subjecting it to heat treatment without drying And a method of treating with a hydrophilizing agent after the heat treatment. Examples of the hydrophilizing agent include hydrogen peroxide water, ozone water, an acetic acid aqueous solution, an aqueous solution of ρΗ4.5 · 9.5, alcohol such as ethanol, and the like. Alternatively, it is possible to generate a hydrophilic silica film by a method S in which ozone is injected during heat treatment.

[0024] The thickness of the silica film 2 (2 ', 12) formed on the main body 1 (1', 11) in this way is not particularly limited, but is about 0.01 to 4 mm 111. And about 0.1 to 2 〃m are more preferable. Thereafter, the silica film 2 (2 ′, 12) is subjected to a surface treatment using a silane coupling agent. As a result, the dental member 4 (4 ′, 14) including the main body 1 (1 ′, 11), the silica film 2 (2 ′, 12), and the silane coupling layer 3 (3 ′, 13) is obtained.

[0025] As the silane coupling agent, those commercially available as dental silane coupling agents can be appropriately used, and the surface treatment method can also be performed by a known method.

Specific examples of silane coupling agents include imperpo porcelain primer (product name, manufactured by Matsukaze), monobond S (product name, manufactured by Ivoclar Vivadent), ReliX ceramic primer (product name, manufactured by 3M ESPE). , GC ceramic primer (product name, manufactured by GC company), Gicera Cosmotech II primer (product name, manufactured by GC company), Tokso ceramic primer (product name, manufactured by Tokama Dental Co.), porcelain liner M (product) Name, manufactured by Sun Medical), combination of porcelain bond activator and clearfill megabond primer (both product names, manufactured by Kuraray Medical), combination of porcelain bond activator and clearfill megabond primer II∑ primer (Product names are all manufactured by Kuraray Medical) Porcelain bond activator one and for 併 of Clearfil Photo Bond (Les, the deviation is also the product name, Kuraray Medical Co., Ltd.) and the like.

[0026] Further, after the polysilazane is converted to silica by an arbitrary method, and before the surface treatment with the silane coupling agent, the silica film 2 (2 ', 12) is irradiated with ultraviolet rays, flame or plasma. It is preferable to carry out. As a result, the effect of improving the adhesiveness according to the present invention can be obtained better.

It is considered that the adhesion between the silica film 2 (2 ′, 12) and the silane coupling layer 3 (3 ′, 13) is improved by performing the treatment by ultraviolet irradiation, flame irradiation or plasma irradiation.

[0027] In addition, when performing flame irradiation or plasma irradiation, the adhesion can be further improved. Therefore, it is performed while spraying fine water droplets of water or hydrogen peroxide water on the irradiated portion, or water Or it is more preferable to carry out in a steam atmosphere with hydrogen peroxide.

[0028] In the present invention, "fine water droplets" refers to mist-like water droplets having a particle diameter of about 0 .; 1 m to 1000 m, preferably in the range of particle diameters of 10 m to 100 m. is there.

The concentration of the hydrogen peroxide solution to be used is not limited as long as the effects of the present invention are not impaired, but a range of 1% to 20% is preferable. [0029] The specific means for generating the fine water droplets or steam of the water or hydrogen peroxide solution is not particularly limited as long as the effects of the present invention are not impaired, but is generally used in the dental field. Can be used. For example, a steam generation unit “MCF-02-300-ST” (trade name) manufactured by Contamination 'Control. Service Co., Ltd. (trade name) can be used to generate water or hydrogen peroxide vapor. is there. Further, in order to spray or spray the fine water droplets, for example, a nozzle “A M6” manufactured by Atmax Co., Ltd. can be used.

[0030] In the present invention, as a specific embodiment indicated by the terms "while spraying fine water droplets" or "under a hydrogen peroxide water vapor atmosphere", by using the above method and apparatus, Irradiating the flame or plasma to the surface of the silica film while introducing minute water droplets or water vapor into the flame in the treatment or into the plasma in the plasma treatment is effective in that the adhesion can be further improved. It is.

[0031] In the ultraviolet irradiation, the silica film is preferably irradiated with ultraviolet light having a light wavelength of 150 nm to 400 nm for 1 minute to 30 minutes.

For the flame irradiation, for example, a commercially available dental medical instrument such as “Handy Torch” (trade name) manufactured by YDM Co., Ltd. can be used. These products can be used to inject flames as a pen-type gas burner by injecting any combustible gas, and can be used not only in the laboratory by dental technicians, but also in dentists. It can also be used in clinical settings.

The treatment time for flame irradiation should be set appropriately according to the type of silica film, silane coupling agent, use in the laboratory by a dental technician, etc., or use in a clinical setting by a dentist. However, 2 to 60 seconds is preferred because it can provide high adhesion.

[0033] For the plasma irradiation, for example, "atmospheric pressure micro-hollow plasma" (trade name) manufactured by NU Eco Engineering Co., Ltd. can be used. When the plasma treatment of the silica film is performed, the effect of improving the adhesiveness according to the present invention can be further enhanced by actions such as surface modification of the silica film, improvement of hydrophilicity, removal of surface deposits and the like. it can.

The processing time of the plasma irradiation is appropriately set within a range that does not impair the effects of the present invention! In order to ensure a determinable force and high adhesiveness, 1 second to 120 seconds is preferable.

[0034] According to the dental member of the present invention, high adhesive strength between the dental member main body and the adherend can be obtained. This is because a silica film generated from polysilazane is provided on the adhesive surface of a dental member body, and the silica film is surface-treated with a silane coupling agent, whereby the adhesive surface of the dental member body and a resin material are provided. This is thought to be due to the improvement in the adhesive strength with resin-based adhesives and adherends that have resin power. In particular, when the material of the dental member body is metal or ceramic, it has been difficult to obtain sufficient adhesive strength between them and the resin material. Therefore, the effect of improving the adhesive strength according to the present invention is great. .

The dental member of the present invention can be easily put to practical use because a high adhesive strength can be obtained by using a resin-based adhesive conventionally used as an adhesive.

The present invention is not limited to the production and mounting of prosthetic devices as shown in Figs. !! to 3, but can be widely applied to similar bonding forms in dental parts. For example, it can be applied to adhesion in repair / restoration of dental parts, and the adhesion strength can be improved.

Example

[0035] The ability to explain the present invention in more detail below using examples The present invention is not limited to these examples.

Examples of the material of the dental component body include stainless steel (SUS304), gold-silver-palladium alloy, gold alloy (18K), and ceramic containing 92% zircoure, depending on the presence or absence of a silica film silane coupling layer produced from polysilazane. In order to investigate the difference in adhesive strength, the following tests were conducted.

[Test Example 1]

First, the upper surface (adhesion surface) of a plate-shaped substrate (15 mm x 15 mm x 3 mm) made of stainless steel (SUS304) is mirror-polished with # 4000 water-resistant abrasive paper, and then the adhering surface is ultra-superposed in an acetone bath. Sonicated.

Next, a coating solution was applied onto the adhesive surface and air-dried for 10 minutes in an atmosphere at 22 ° C. As the coating solution, a product prepared by AZ Electronic Materials Co., Ltd., Aquamica NP 110 (product name, xylene solution of perhydropolysilazane) diluted with xylene to a perhydropolysilazane concentration of 10% by mass was used. . Thereafter, the mixture was heat-treated in an oven at 300 ° C. for 3 hours and then allowed to cool at room temperature.

Using a Fourier transform infrared spectrophotometer (manufactured by Shimadzu Corporation, product name: FT-IR8000), the film formed on the adhesive surface of the base material in the wave number range of 4600 to 650 cm- ^{1 by} the ATR method. FT—IR spectrum was measured. The results are shown in Fig. 4. An index of silica conversion

The intensity of the absorption peak attributed to Si—N in the vicinity of SSOcnT ¹ indicating the residual unreacted perhydropolysilazane was examined. As a result, peaks near lOeOcnT ¹ and SOOcnT ¹ were prominent, and no peaks were found near 830c π ¹ . From this, it was confirmed that the film formed on the adhesion surface was a silica film. The thickness of the silica film was 0.85 mm.

Further, a GC ceramic primer (product name, manufactured by GS Co., Ltd.) as a silane coupling agent was applied to the adhesive surface on which the silica film was formed, and dried to obtain a test piece.

[0037] (Test Example 2)

As in Test Example 1, except that the base material was changed to a gold-silver-palladium alloy (“Castwell (Gold 12%) MC” (Gishi Co., Ltd.)). A test piece was prepared. The thickness of the silica film was 0.85 mm.

[0038] (Test Example 3)

A test piece was prepared in the same manner as in Test Example 1 except that the material of the base material was changed to 18K gold alloy in Test Example 1. The thickness of the silica film was 0.85 111.

[0039] (Test Example 4)

In Test Example 1, the material of the base material was changed to a ceramic containing 92% zirconia. In addition, the coating solution was prepared by diluting AZ Electronic Materials Co., Ltd., Aquamica NL-120 (product name, perhydropolysilazane dibutyl ether solution) with dibutyl ether to a perhydropolysilazane concentration of 5% by mass. The oven heat treatment conditions were changed to 500 ° C for 3 hours. Otherwise, test pieces were prepared in the same manner as in Test Example 1. The thickness of the silica film was 0.18 mm.

[0040] (Test Example 5)

In Test Example 4, after the heat treatment and before applying the silane coupling agent, the silica film was irradiated with ultraviolet rays of 185 nm for 10 minutes. Otherwise, the test piece was the same as Test Example 4. Was made.

[0041] (Comparative test example;! To 4)

In each of the above test examples;! To 4, a sample that was not subjected to formation of a silica film and surface treatment with a silane coupling agent was prepared as a comparative test piece. That is, in the same manner as in Test Example 1, the upper surface (adhesion surface) of the base material was mirror-polished, and the adhesion surface was simply ultrasonically cleaned in an acetone bath to obtain a comparative test piece.

[0042] <Evaluation of adhesive strength>

The adhesive strength of the test pieces obtained in Test Examples 1 to 5 and Comparative Test Examples 1 to 4 was evaluated by the following method.

5 and 6 are schematic diagrams for explaining the method for evaluating the adhesive strength. In the figure, reference numeral 21 denotes a base material (test piece), and 21a denotes an adhesive surface of the base material.

First, as shown in FIG. 5, an adhesive tape 22 having a through hole 22a having a diameter of 3 mm in the center was pasted on the adhesive surface 21a of a base material (test piece) 21. On the other hand, 0.4 g of resin cement (product name: GC LINKMA X, manufactured by GC Corporation) was piled on the lower surface 23a of a cylindrical methanol rod 23 (material: SUS304) having a diameter of 5 mm. Then, the lower surface 23a of the metal rod 23 and the adhesive surface 21a of the base material 21 were pressed against each other so as to sandwich the through hole 22a of the adhesive tape 22, and left at room temperature for 30 minutes to cure the resin cement. In this way, in the through hole 22a of the adhesive tape 22, the lower surface 23a of the metal rod and the adhesive surface 21a of the base material were bonded via the resin cement.

Next, after the metal rod 23 and the base material 21 were immersed in distilled water for 24 hours in a 37 ° C constant temperature bath, the direct tensile test device 24 (manufactured by Shimadzu Corporation) shown in Fig. 6 was stored. , Product name: AGS-500), and tensile strength (unit: MPa) was measured by pulling the metal rod 23 upward. The crosshead speed was 1. Omm / min, and the maximum tensile strength before fracture occurred was recorded. Table 1 shows the measurement results. The value of the measurement result is an average value of five test pieces prepared under the same conditions.

[0043] [Table 1] fe resin cocoons | Silica film | Adhesive strength (MPa)

Test cases 1 Yes

Comparison example 1 J No! S.7S

Test Example 2 Gold-Silver Rashi'um Alloy] Yes | 18.37

Comparative example 2 / I No I 6.3?

Difficult example 3 18K gold food J% `` 15.71

Male, example 3 None I 1.04

Contains zirconia |

Test example 4

Ceramics * | 1S.3

Comparison Example 4

Test example 5 Yes! 18,5

[0044] From the results of Table 1, Test Examples 1 to 5 in which a silica film was formed on the adhesive surface and treated with a silane coupling agent were compared with Comparative Test Examples 1 to 4 in which a silica film was not formed, respectively. The adhesive strength was remarkably improved, and good adhesive strength of 15 MPa or more was obtained in all cases. Industrial applicability

[0045] The dental member according to the present invention is extremely high in that it can be used in the field of dentistry and has industrial applicability. In addition, according to the method for producing a dental member according to the present invention, a commonly used dental member can be firmly adhered to an adherend such as a tooth, and used in a laboratory such as a dental technician. Or it can be used in clinical practice by dentists, so it has very high availability in the industry.

Claims

The scope of the claims

[1] A dental member, characterized in that a silica film generated from polysilazane is provided on the dental member body, and the silica film is surface-treated with a silane coupling agent.

[2] A step of applying a polysilazane-containing coating solution on a dental member body, then converting the polysilazane to silica to form a silica film, and a step of surface-treating the silica film with a silane coupling agent The manufacturing method of the dental member characterized by having.

3. The method for producing a dental member according to claim 2, wherein the silica film is subjected to surface treatment with the silane coupling agent after being irradiated with ultraviolet rays.

[4] The dental treatment according to claim 2, wherein the silica film is subjected to a surface treatment with the silane coupling agent after being irradiated with a flame while spraying fine water droplets of water or in a water vapor atmosphere. Manufacturing method of member.

[5] The silica film is subjected to a surface treatment with the silane coupling agent after being irradiated with a flame while spraying fine water droplets of hydrogen peroxide solution or in a vapor atmosphere of hydrogen peroxide solution. The method for producing a dental member according to claim 2.

6. The dental treatment according to claim 2, wherein the silica film is surface-treated with the silane coupling agent after being irradiated with plasma while spraying fine water droplets of water or in a water vapor atmosphere. Manufacturing method of member.

[7] The silica film is subjected to surface treatment with the silane coupling agent after being irradiated with plasma while spraying fine water droplets of hydrogen peroxide solution or in a vapor atmosphere of hydrogen peroxide solution. The method for producing a dental member according to claim 2.