CN102994946A - Method for enhancing bonding strength of dental titanium porcelain through depositing nanometer niobium nitride - Google Patents
Method for enhancing bonding strength of dental titanium porcelain through depositing nanometer niobium nitride Download PDFInfo
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- CN102994946A CN102994946A CN2011102690309A CN201110269030A CN102994946A CN 102994946 A CN102994946 A CN 102994946A CN 2011102690309 A CN2011102690309 A CN 2011102690309A CN 201110269030 A CN201110269030 A CN 201110269030A CN 102994946 A CN102994946 A CN 102994946A
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Abstract
The invention provides a method for enhancing the bonding strength of dental titanium porcelain through depositing nanometer niobium nitride. The method comprises the following steps: 1, screening a pure titanium substrate having no casting defects, pre-treating the pure titanium substrate, sandblasting the pure titanium substrate under a certain pressure, cleaning the pure titanium substrate after sandblasting ending, and blowing the pure titanium substrate by pure nitrogen to dryness; 2, depositing nanometer niobium nitride on the surface of the pure titanium substrate obtained after treating in step 1 through a depositing process; and 3, carrying out porcelain sintering of the pure titanium substrate subjected to the depositing treatment in a porcelain furnace by utilizing porcelain powder to obtain a porcelain fused titanium material. The method has the advantages of simple operation, inhibition of the oxidation of pure titanium at a porcelain sintering temperature, reaching of a titanium porcelain bonding strength enhancing purpose without influencing the aesthetic effect, convenient relevant material and equipment obtaining, good clinical application prospect, and high practical application value.
Description
Technical field
The present invention relates to a kind of method that strengthens titanium porcelain bonding, especially a kind of method of enhancing dentistry titanium porcelain bonding of the depositing nano level niobium nitride that is applied to the dental care field.
Background technology
The pfm material is the most fixing dental case of present clinical application, but wherein sensitization and the bio-toxicity of the metallic element such as nickel may cause some adverse consequencess.Pure titanium material is owing to have good biocompatibility, erosion resistance; suitable physicals and chemical property are widely used at biomedical sector; its low density and thermal conductivity; with other metals and alloy ratio; it is protected dental pulp, avoids the effect of caloric stimulation more obvious, is considered to make the desired metallic material of Metal-porcelain dummy.
The combination of titanium in dentistry dummy and porcelain belongs to Chemical bond, and its bonding force mainly depends on the bonding force of zone of oxidation itself, porcelain and zone of oxidation, zone of oxidation and metal titanium.In the past, there was oxidation behavior in pure-titanium prosthesis under the porcelain sintering temperature, and blocked up, the unprotect of formation and the poor oxide film of tack are considered to cause the major cause of titanium porcelain repairing failure.In recent years, the development of titanium low fusing porcelain powder makes the titanium porcelain reparation become possibility, however, has not yet to see the Long-term clinical report of relevant titanium porcelain dummy.Short-term observation shows that the mortality of titanium porcelain dummy is high, and it unsuccessfully shows as, and porcelain splits and porcelain facing partly or entirely comes off.As seen, how to improve titanium porcelain bonding and be still a problem that waits to solve.
Summary of the invention
The object of the present invention is to provide a kind of method that strengthens titanium porcelain bonding, it is by depositing nano level niobium nitride between pure titanium substrate and porcelain and then increased the resistance of pure titanium substrate oxidation, has suppressed the formation of oxide film, has improved the bonding strength of titanium and porcelain.
For achieving the above object, a kind of depositing nano level niobium nitride of the present invention strengthens the method for dentistry titanium porcelain bonding, and it comprises the steps:
A. the pure titanium substrate of dental is carried out surface preparation;
B. at pretreated pure titanium substrate surface depositing nano level niobium nitride film;
C. the pure titanium substrate after using the porcelain powder to film forming carries out the porcelain sintering in porcelain oven body, to obtain the molten attached titanium material of porcelain.
As a further improvement on the present invention, described step a comprises: screening is without the pure titanium substrate of casting flaw, remove the impurity of described pure titanium substrate surface, then be exposed in the air, make the passivation of pure titanium substrate, passivation time is controlled at 10 minutes, after finishing, cleaned 5 minutes with heat steam passivating process, and then with acetone ultrasonic cleaning 15 minutes, to be cleaned complete, with pure nitrogen gas pure titanium substrate is dried up; Control pressure is under the condition of 2 bar (bar), and described pure titanium substrate is carried out sandblast, and sandblast is cleaned pure titanium substrate 5 minutes with hot steam after finishing, and uses the acetone ultrasonic cleaning 15 minutes again, dries up with pure nitrogen gas at last.
As a further improvement on the present invention, whether screening utilizes X ray to exist defective to survey to pure titanium substrate inside during without the pure titanium substrate of casting flaw.
As a further improvement on the present invention, the method for the pure titanium substrate surface of described removal impurity comprises that employing wolfram varbide bistrique polishes pure titanium substrate, and wherein wolfram varbide bistrique rotating speed is less than or equal to 15000rpm.
As a further improvement on the present invention, Al is adopted in described sandblast
2O
3, sand spit and pure titanium substrate distance are 10mm, the sandblast angle is 45 °.
As a further improvement on the present invention, the method for described depositing nano level niobium nitride film comprises magnetron sputtering method or ion beam assisted depositing method or pulsed laser deposition.
As a further improvement on the present invention, described magnetron sputtering method uses the magnetically controlled DC sputtering instrument, and working conditions is: forvacuum degree 6.0 * 10
-6Pa, air pressure 0.3Pa, sputtering power 350w, depositing temperature normal temperature, the quiet 15 minutes time, working gas is Ar and N
2Mixed gas, Ar/N is than for 6:1; And take pure titanium substrate as negative electrode, the niobium target is anode, and the distance of pure titanium substrate and niobium target is 60mm, and whole sputter procedure is utilized circulating water.
As a further improvement on the present invention, before utilizing described magnetron sputtering method depositing nano level niobium nitride film, with Ar pure titanium substrate is carried out reverse sputtering first and clean, scavenging period is 10 minutes.
Compared with prior art, the invention has the beneficial effects as follows: by the nano level niobium nitride film at titanium in dentistry substrate surface deposition even compact, suppress the oxidation behavior of pure titanium under the porcelain sintering temperature, and reached the purpose that strengthens titanium porcelain bonding on the basis that does not affect aesthetic effect.In addition, associated materials of the present invention and equipment obtain comparatively convenient, and is easy and simple to handle, has good potential applicability in clinical practice and higher actual application value.
Description of drawings
Fig. 1 is the XRD analysis result of the nano level niobium nitride film of the material prepared in the embodiment of method of the present invention;
Fig. 2 is the SEM observations of the nano level niobium nitride film of the material prepared in the embodiment of method of the present invention;
Fig. 3 prepares the not SEM observations of the titanium porcelain bonding interface of cvd nitride niobium pentoxide film in one embodiment of method of the present invention;
Fig. 4 is the SEM observations of the titanium porcelain bonding interface of the cvd nitride niobium pentoxide film prepared in the embodiment of method of the present invention.
Embodiment
Describe the present invention below with reference to each embodiment.One of main method of the depositing nano level niobium nitride film that will relate in the following embodiment of paper---magnetron sputtering method.The ultimate principle of magnetron sputtering is to utilize plasma body in the sputter mixed gas under the effect of electric field and alternating magnetic field, the high-energy particle bombardment target material surface that is accelerated, after the energy exchange, the atom of target material surface breaks away from former lattice and overflows, and high energy particle is transferred to matrix surface and film forming.Magnetron sputtering has now become the preferred option of plated film industrial circle with advantages such as sputtering raste is high, base material temperature is low, the film base is combined, device performance is stable, convenient operation and control.In the technical program, adopt the magnetically controlled DC sputtering instrument as reaction kit, take pure titanium substrate as negative electrode, with the niobium target as anode, make the niobium nitride particle in the effect deposit of the electric field of magnetically controlled DC sputtering instrument and alternating magnetic field on pure titanium surface, form the niobium nitride film.
Because niobium nitride has the sodium chloride crystal structure, thermostability and chemical stability are high, anti-neutron radiation, it is good superconducting material, and niobium nitride hardness is high, high, wear-resistant, the resistance to chemical attack and high temperature resistant of fusing point, and these character are so that niobium nitride is suitable for the material as the resistance of oxidation that improves titanium.
The niobium element has relatively large diffusibility and reactive behavior in high-temperature oxidation environment, can be formed with on the surface the fine and close responding layer of the oxide compound of multiple valence state niobium, this zone of oxidation has the function of similar people " palm cocoon ", can effectively stop zone of oxidation cracking and deep oxidation, show to a certain extent the anti-oxidant behavior of self-adaptation, and then improved the resistance of oxidation of titanium, strengthened the bonding strength of titanium porcelain.
Although the deposition method in the technical scheme can adopt ion beam assisted depositing method or pulsed laser deposition, in the present embodiment, the deposition method of niobium nitride adopts magnetron sputtering method, specifically comprises the steps:
A. utilize X ray whether to exist defective to survey to pure titanium substrate inside, screening is without the pure titanium substrate of casting flaw, remove its surperficial impurity with the wolfram varbide bistrique, the bistrique rotating speed should be lower than 15000rpm, then is exposed in the air, make the passivation of pure titanium substrate, passivation time is controlled at 10 minutes, after finishing, cleaned 5 minutes with heat steam passivating process, and then with acetone ultrasonic cleaning 15 minutes, to be cleaned complete, with pure nitrogen gas pure titanium substrate is dried up.Control pressure is under the condition of 2 bar (bar), uses 120 μ mAl
2O
3Particle carries out sandblast to described pure titanium substrate, and sand spit and pure titanium substrate distance are 10mm, and the sandblast angle is 45 °, and sandblast is cleaned pure titanium substrate 5 minutes with hot steam after finishing, and uses the acetone ultrasonic cleaning 15 minutes again, dries up with pure nitrogen gas at last.
B. utilizing magnetron sputtering method depositing nano level niobium nitride through the pure titanium substrate surface after a step process, note, will carry out reverse sputtering to pure titanium substrate with Ar first before deposition cleans, scavenging period is 10 minutes, and then carry out sputter, described magnetron sputtering method utilizes the magnetically controlled DC sputtering instrument, and working conditions is: forvacuum degree 6.0 * 10
-6Pa, air pressure 0.3Pa, sputtering power 350w, depositing temperature normal temperature, the quiet 15 minutes time, working gas is Ar and N
2Mixed gas, Ar/N is than for 6:1; And take pure titanium substrate as negative electrode, the niobium target is anode, and the distance of pure titanium substrate and niobium target is 60mm, and whole sputter procedure is utilized circulating water.
C. then utilize the porcelain powder that the pure titanium substrate through depositing treatment is carried out the porcelain sintering in porcelain oven body, obtain the molten attached titanium material of porcelain.The program of porcelain sintering is decided according to the porcelain powder using method of relevant brand.
At last, the molten attached titanium material of the porcelain that obtains is carried out performance test.The method of performance test has X-ray diffraction (XRD) to analyze or scanning electronic microscope (SEM) is analyzed or the X-ray energy spectrum (EDS) of scanning electron microscope is analyzed or digit microscope (DM) is analyzed or roughness mutation analysis or bonding strength analysis, these performance test analysis methods can select to be suitable for one or more as the case may be, thus many-sided structure and characteristic that characterizes the material of preparation.
The present invention will be further described below in conjunction with specific embodiment.
Embodiment one:
Utilize X ray screening without 30 of the pure titanium substrates of casting flaw, its specification is 25mm * 3mm * 0.5mm, removes surface impurity with the wolfram varbide bistrique, pure titanium substrate is carried out polished finish, bistrique rotating speed≤15000rpm.After polished processing finishes, place air to carry out self-passivation pure titanium substrate and process, passivation time is 10 minutes, then pure titanium substrate is cleaned, and cleans 5 minutes with hot steam first, uses the acetone ultrasonic cleaning 15 minutes again, dries up with pure nitrogen gas at last.
Under 2bar pressure, with 120 μ mAl
2O
3Particle carries out sandblasting to pure titanium substrate, and the distance of sand spit and pure titanium substrate is 10mm, and the sandblast angle is 45 °, and the sandblast time is 5 minutes.Sandblasting is cleaned once pure titanium substrate after finishing again, and still cleans 5 minutes with hot steam first, uses the acetone ultrasonic cleaning 15 minutes again, dries up with pure nitrogen gas at last.
To carry out reverse sputtering with Ar through the pure titanium substrate that above-mentioned steps was processed cleans, for magnetron sputtering method cvd nitride niobium is afterwards prepared, scavenging period is 10 minutes, clean complete, place the magnetically controlled DC sputtering instrument to carry out the magnetron sputtering deposition niobium nitride pure titanium substrate, working gas is the mixed gas of Ar and N2, and as negative electrode, the niobium target is as anode with pure titanium substrate, pure titanium substrate and niobium range are from being 60 mm, forvacuum degree 6.0 * 10-6 Pa, operating air pressure 0.3 Pa, sputtering power 350 w, Ar/N2 is than being 6:1, depositing temperature is normal temperature, depositing time 15 minutes, and whole sputter procedure is utilized circulating water.
At last, (8mm * 3mm) locates to carry out the porcelain sintering in substrate center to choose VITA TITANKERAMIK porcelain powder, the program of porcelain sintering is decided according to the porcelain powder using method of relevant brand, chooses Multimant Touch porcelain oven body in this embodiment as the porcelain agglomerating plant.
Namely obtain the molten attached titanium material of porcelain through the porcelain sintering, the superiority with respect to prior art of the product that obtains for the preparation method who proves by the technical program is carried out every test analysis to product, to characterize its performance and internal structure.
As shown in Figure 1, reflected the XRD analysis result of nano silicon nitride niobium pentoxide film, this result shows that the niobium nitride that generates under the magnetron sputtering condition is the Emission in Cubic crystal, there are (111), (200), the different crystallographic orientations of (220) and (222), XRD result has shown titanium and Al simultaneously
2O
3Existence.
As shown in Figure 2, be the result who utilizes SEM that the surface topography of nano silicon nitride niobium pentoxide film is observed, this result shows that nano level niobium nitride uniform particles is distributed in coarse Al
2O
3The surface has no obvious crack or damaged, niobium nitride and Al
2O
3Surface bonding is good.
As shown in Figure 4, what this figure reflected is to utilize SEM to observe the result of the titanium porcelain bonding interface of depositing nano niobium nitride film, can find out that from this result combination is comparatively good between titanium-porcelain, exists several to be dispersed in hole, has no obvious crackle and porcelain and strips off phenomenon.
Embodiment two:
This embodiment is identical with embodiment one for the processing mode in the early stage of pure titanium substrate, no longer give unnecessary details herein, embodiment two is with the difference of embodiment one: pure titanium substrate surface does not carry out the deposition of niobium nitride, directly to carrying out the porcelain sintering through dry pure titanium substrate after sandblasting and the cleaning, the porcelain sintering procedure carries out with reference to the regulation of the specification sheets of selected porcelain powder.
Then the product that embodiment two is obtained carry out performance test.
As shown in Figure 3, it is to utilize SEM to the observations of the titanium porcelain bonding interface of cvd nitride niobium pentoxide film not, can see that from this result more and large hole and crackle are dispersed in distribution, illustrates that the titanium porcelain bonding through the niobium nitride deposition is not high.
The purpose of design of embodiment two is in order to compare with embodiment one, the superiority of technical solution of the present invention better to be described.
Simultaneously, the X-ray energy spectrum (EDS) by scanning electron microscope is analyzed the situation of oxygen level among the embodiment one and two, by analysis titanium-Al as can be known
2O
3In both sides, the interface element of-niobium nitride-porcelain, porcelain side oxygen level is 43.0% among the embodiment one, and pure titanium side is 5.6%; Porcelain side oxygen level is 44.8% among the embodiment two, and pure titanium side is 15.9%, the result shows that magnetron sputtering niobium nitride coating has stopped the diffusion of oxygen to titanium, has effectively suppressed the oxidation of titanium.
The recycling roughness measuring instrument is analyzed the surfaceness of pure titanium substrate variation before and after the film forming among embodiment one and the embodiment two, (8mm * 3mm) chooses 5 zones at random in pure titanium substrate center, analytical results is as follows: polish pure titanium substrate roughness and be (0.1292 ± 0.0106) μ m, (Al among the embodiment two
2O
3) the group roughness be (1.8634 ± 0.1048) μ m, among the embodiment one (Al2O3+ niobium nitride) to organize roughness be (2.3304 ± 0.0805) μ m.By statistics Epidemiological Analysis as can be known, Al
2O
3Significantly increased the roughness on pure titanium surface, the nano silicon nitride niobium has increased the roughness on pure titanium surface.This result shows that the nano silicon nitride niobium has increased the roughness of pure titanium substrate surface, has increased the contact area of porcelain powder and pure titanium, makes the porcelain powder that better wettability be arranged, and forms better mechanical keying action behind sintering.
At last, by ISO9693 1999 standards the molten attached titanium material of porcelain is carried out three point bending test and measure bonding strength, use formula τ
b=k * F
FailCalculate the three-point bending bonding strength (k=4.6 in the formula) between titanium porcelain, adopt the SPSS17.0 statistical software to carry out statistical procedures.It is as follows that each organizes titanium porcelain bonding: (titanium/Al among the embodiment one
2O
3/ niobium nitride/porcelain) bonding strength is (43.112 ± 0.586) MPa; (titanium/Al among the embodiment two
2O
3/ porcelain) bonding strength is (27.242 ± 0.752) MPa, has reached to require titanium/porcelain bonding strength Schwellenwert 25MPa among the ISO9693 1999.The cvd nitride niobium coating by whether is to (titanium/Al among the embodiment one
2O
3/ niobium nitride/porcelain) (titanium/Al and among the embodiment two
2O
3/ porcelain) t that carries out single factor Group Design measurement data checks (t=52.6404, P=0.0000), and difference has statistical significance.The result shows that magnetron sputtering nano silicon nitride niobium can improve the bonding strength of titanium-low fusing porcelain.
Claims (8)
1. the method for a depositing nano level niobium nitride enhancing dentistry titanium porcelain bonding is characterized in that the method comprises the steps:
A. the pure titanium substrate of dental is carried out surface preparation;
B. at pretreated pure titanium substrate surface depositing nano level niobium nitride film;
C. the pure titanium substrate after using the porcelain powder to film forming carries out the porcelain sintering in porcelain oven body, to obtain the molten attached titanium material of porcelain.
2. method according to claim 1, it is characterized in that, described step a comprises: screening is removed the impurity of described pure titanium substrate surface without the pure titanium substrate of casting flaw, then is exposed in the air, make the passivation of pure titanium substrate, passivation time is controlled at 10 minutes, after finishing, cleaned 5 minutes with heat steam passivating process, and then with acetone ultrasonic cleaning 15 minutes, to be cleaned complete, with pure nitrogen gas pure titanium substrate is dried up; Control pressure is under the condition of 2 bar (bar), and described pure titanium substrate is carried out sandblast, and sandblast is cleaned pure titanium substrate 5 minutes with hot steam after finishing, and uses the acetone ultrasonic cleaning 15 minutes again, dries up with pure nitrogen gas at last.
3. method according to claim 2 is characterized in that, whether screening utilizes X ray to exist defective to survey to pure titanium substrate inside during without the pure titanium substrate of casting flaw.
4. method according to claim 2 is characterized in that, the method for the pure titanium substrate surface of described removal impurity comprises that employing wolfram varbide bistrique polishes pure titanium substrate, and wherein wolfram varbide bistrique rotating speed is less than or equal to 15000rpm.
5. method according to claim 2 is characterized in that: described sandblast employing Al
2O
3, sand spit and pure titanium substrate distance are 10mm, the sandblast angle is 45 °.
6. method according to claim 1 is characterized in that, the method for described depositing nano level niobium nitride film comprises magnetron sputtering method or ion beam assisted depositing method or pulsed laser deposition.
7. method according to claim 6 is characterized in that: described magnetron sputtering method uses the magnetically controlled DC sputtering instrument, and working conditions is: forvacuum degree 6.0 * 10
-6Pa, air pressure 0.3Pa, sputtering power 350w, depositing temperature normal temperature, the quiet 15 minutes time, working gas is Ar and N
2Mixed gas, Ar/N is than for 6:1; And take pure titanium substrate as negative electrode, the niobium target is anode, and the distance of pure titanium substrate and niobium target is 60mm, and whole sputter procedure is utilized circulating water.
8. method according to claim 7 is characterized in that: before utilizing described magnetron sputtering method depositing nano level niobium nitride film, with Ar pure titanium substrate is carried out reverse sputtering first and clean, scavenging period is 10 minutes.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104029435A (en) * | 2014-06-10 | 2014-09-10 | 上海理工大学 | NbN/WS2 multilayer coating with high hardness and low friction coefficient and preparation method thereof |
| CN116949410A (en) * | 2023-09-20 | 2023-10-27 | 西安聚能医工科技有限公司 | Method for magnetron sputtering coating on surface of alloy substrate, product and application thereof |
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| US4726890A (en) * | 1985-08-12 | 1988-02-23 | The United States Of America As Represented By The Administrator Of The National Aeronautics And Space Administration | Method of producing high Tc superconducting NbN films |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104029435A (en) * | 2014-06-10 | 2014-09-10 | 上海理工大学 | NbN/WS2 multilayer coating with high hardness and low friction coefficient and preparation method thereof |
| CN104029435B (en) * | 2014-06-10 | 2016-04-27 | 上海理工大学 | A kind of NbN/WS with high rigidity and low-friction coefficient 2laminated coating and preparation method thereof |
| CN116949410A (en) * | 2023-09-20 | 2023-10-27 | 西安聚能医工科技有限公司 | Method for magnetron sputtering coating on surface of alloy substrate, product and application thereof |
| CN116949410B (en) * | 2023-09-20 | 2023-12-19 | 西安聚能医工科技有限公司 | Method for magnetron sputtering coating on surface of alloy substrate, product and application thereof |
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Application publication date: 20130327 |