CN116789447A - Zirconia dental floss material with thin-wall structure and preparation method thereof - Google Patents

Zirconia dental floss material with thin-wall structure and preparation method thereof Download PDF

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CN116789447A
CN116789447A CN202310783240.2A CN202310783240A CN116789447A CN 116789447 A CN116789447 A CN 116789447A CN 202310783240 A CN202310783240 A CN 202310783240A CN 116789447 A CN116789447 A CN 116789447A
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dental floss
zirconia
parts
blank
thin
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CN116789447B (en
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刘耀
吴杰华
杨华杰
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Jiangxi Jinshi 3d Intelligent Manufacturing Technology Co ltd
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Jiangxi Jinshi 3d Intelligent Manufacturing Technology Co ltd
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Abstract

The application is suitable for the technical field of dental materials, and provides a zirconia dental floss material with a thin-wall structure and a preparation method thereof. In addition, the zirconia powder subjected to presintered treatment is fully filled in the concave surface on the inner side of the curved surface green body, so that the uniform heating of the green body can be ensured, cracks are avoided, and the quality of a finished product is improved.

Description

Zirconia dental floss material with thin-wall structure and preparation method thereof
Technical Field
The application belongs to the technical field of dental materials, and particularly relates to a zirconia dental floss material with a thin-wall structure and a preparation method thereof.
Background
Zirconium oxide is used as a common metal oxide, has the advantages of high hardness, high strength, corrosion resistance, high biocompatibility and the like, and is widely applied to the fields of orthopedic implants, dental restorations and the like as a biological material. However, the traditional zirconia ceramics have long processing period and high processing technology, so that the price of zirconia biomaterials customized for individuals is high, and the further application of the zirconia biomaterials is affected.
Modern society people pay more and more attention to oral health, the oral medical industry rapidly develops, and more people put forth personalized demands on dental restoration. The denture material has enough high customization freedom degree while meeting the basic mechanical property and biological property, and can keep consistent with the shape of the original teeth or meet the individual customization requirement of users. This presents further challenges to zirconia forming processes, especially in the case of thin-walled structures for dental floss products that are difficult to obtain by conventional manufacturing processes, and present significant processing difficulties and high costs.
The DLP technology is a 3D printing technology based on a photo-curing principle, a model with a specific shape can be quickly prepared according to a computer model, and the zirconia ceramic tooth is obtained by degreasing, sintering and removing resin components. Compared with SLA and sinking DLP technologies, the lifting DLP has the advantages of less needed slurry, high printing speed and low equipment cost, and is beneficial to popularization and application of zirconia porcelain teeth. However, the existing DLP slurry for preparing the zirconia dental floss material has insufficient blank strength to adapt to the lifting DLP forming process and low degreasing efficiency, and is not beneficial to the application and promotion of the zirconia ceramic dental floss.
Disclosure of Invention
The embodiment of the application provides a preparation method of a zirconia dental floss material with a thin-wall structure, and aims to solve the problems that the strength of a blank body is insufficient to adapt to a lifting DLP forming process and the degreasing efficiency is low in the existing DLP slurry for preparing the zirconia dental floss material.
The embodiment of the application is realized in such a way that the preparation method of the zirconia dental floss material with the thin-wall structure comprises the following steps:
mixing 30-50 parts of epoxy acrylate, 15-25 parts of hydroxyethyl acrylate, 15-25 parts of trimethylolpropane triglycidyl ether, 15-25 parts of 1, 6-hexanediol diacrylate, 0.1-0.5 part of diphenyl- (2, 4, 6-trimethyl benzoyl) phosphorus oxide, 2-8 parts of dispersing agent, 2-6 parts of liquid paraffin and 0.5-1.5 parts of defoamer in a vacuum stirring manner to obtain a photo-curing resin premix;
ball milling and mixing zirconia powder and the photo-curing resin premix, and stirring in vacuum to obtain DLP photo-curing slurry;
printing by using the DLP photo-curing slurry to obtain a dental socket blank, filling all the concave surfaces on the inner side of the dental socket blank with pre-sintered zirconia powder, degreasing at 100-500 ℃ at a heating rate of 0.1-10 ℃/min, heating to 1000-1200 ℃ after degreasing, and preserving heat for 1-3 hours;
after degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank body by using air flow, and sintering to obtain the zirconia dental floss material with the thin-wall structure.
The embodiment of the application also provides the zirconia dental floss material with the thin-wall structure, which is prepared by the preparation method of the zirconia dental floss material with the thin-wall structure.
According to the preparation method of the zirconia dental floss material with the thin-wall structure, the mass ratio of epoxy acrylate, hydroxyethyl acrylate, trimethylolpropane triglycidyl ether and 1, 6-hexanediol diacrylate is optimized, so that each component of a blank body can be discharged rapidly in stages during degreasing, meanwhile, the added liquid paraffin can improve the fluidity of slurry, slurry sedimentation is prevented, holes are formed in the initial degreasing stage, an escape channel is provided for gas decomposed by the subsequent components, and the blank body can be subjected to ultrasonic cleaning due to optimization of the slurry, so that the residual slurry can be conveniently and efficiently removed. In addition, the zirconia powder subjected to presintered treatment is fully filled in the concave surface on the inner side of the curved surface green body, so that the uniform heating of the green body can be ensured, cracks are avoided, and the quality of a finished product is improved.
Detailed Description
The present application will be described in further detail with reference to specific embodiments in order to make the objects, technical solutions and advantages of the present application more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the application.
The embodiment of the application provides a preparation method of a zirconia dental floss material with a thin-wall structure, which comprises the following steps:
step S1: mixing 30-50 parts of epoxy acrylate, 15-25 parts of hydroxyethyl acrylate, 15-25 parts of trimethylolpropane triglycidyl ether, 15-25 parts of 1, 6-hexanediol diacrylate, 0.1-0.5 part of diphenyl- (2, 4, 6-trimethyl benzoyl) phosphorus oxide, 2-8 parts of dispersing agent, 2-6 parts of liquid paraffin and 0.5-1.5 parts of defoamer by vacuum stirring to obtain the photo-curing resin premix.
In the embodiment of the application, the components can be rapidly discharged in stages during degreasing by optimizing the mass ratio of the epoxy acrylate, the hydroxyethyl acrylate, the trimethylolpropane triglycidyl ether and the 1, 6-hexanediol diacrylate, so that the mechanical property of the obtained zirconia dental floss material with the thin-wall structure is improved. Wherein, when the mass ratio of the epoxy acrylate to the hydroxyethyl acrylate to the trimethylolpropane triglycidyl ether to the 1, 6-hexanediol diacrylate is 2:1:1:1, the strength of the zirconia dental floss material with the thin-wall structure is better.
In a preferred embodiment of the present application, the pre-mixed liquid of the photo-curable resin comprises the following raw materials in parts by weight:
40 parts of epoxy acrylate, 20 parts of hydroxyethyl acrylate, 20 parts of trimethylolpropane triglycidyl ether, 20 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent, 4 parts of liquid paraffin and 1 part of defoamer.
In an embodiment of the present application, the dispersant is one or more of EFKA4703, solsperse AC7570, solsperse 41000.
In the embodiment of the application, the defoamer is one or more of B-0846, B-0847, SN-9228 and B-0848 in any proportion.
In an embodiment of the application, the liquid paraffin is provided by a micin reagent.
Step S2: and performing ball milling mixing treatment on the zirconia powder and the photo-curing resin premix, and performing vacuum stirring to obtain DLP photo-curing slurry.
In an embodiment of the present application, the zirconia powder is a near spherical powder having an average particle diameter of 300 to 400 nm.
Step S3: printing by using the DLP photo-curing slurry to obtain a dental floss blank, filling all the concave surfaces on the inner side of the dental floss blank with pre-sintered zirconia powder, degreasing at 100-500 ℃ at a heating rate of 0.1-10 ℃/min, heating to 1000-1200 ℃ after degreasing, and preserving heat for 1-3h.
In the embodiment of the application, the zirconia powder subjected to the presintered treatment is filled in the concave surface of the inner side of the dental socket blank body, specifically:
placing the dental floss blank into a corundum square boat, paving zirconia powder subjected to presintered treatment in the corundum square boat, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; and (3) placing the tooth surface of the dental floss blank upwards into a corundum ark, so that the concave surface on the inner side of the dental floss is fully filled with the zirconia powder subjected to presintered treatment.
In an embodiment of the present application, the pre-sintered zirconia powder is:
heating micrometer zirconia powder to 1100-1300 ℃ and calcining for 3-5h, grinding after calcining, sieving with a 40-50 mesh screen, sieving to remove oversized particles, sieving with a 80-90 mesh screen to remove fine powder, and obtaining the powder on the 80-90 mesh screen, namely the zirconia powder after presintered treatment. According to the application, the dental floss blank is filled with the micron-sized zirconia subjected to presintered treatment, so that the blank can be uniformly heated, cracks are avoided, the quality of a finished product is improved, and the degreasing efficiency is improved; it is noted that the particle fineness of the zirconia powder needs to be strictly controlled, and an excessively high particle fineness tends to cause some cracking of the product, while an excessively low particle fineness is disadvantageous for degreasing efficiency, and the particle fineness is preferably 30 to 50 μm. In addition, the zirconia powder pre-sintered at a specific temperature is used as the filling powder of the dental floss body, so that the degreasing efficiency is greatly improved, if the zirconia powder which is not pre-sintered is used as the filling powder of the dental floss body, the degreasing treatment is only carried out at a low temperature rising rate (0.2-0.5 ℃/min), otherwise, the performance of the obtained product is greatly reduced, and the dental floss body is easy to crack and the yield is reduced.
In the embodiment of the application, before the concave surface on the inner side of the dental socket blank is fully filled with the zirconia powder subjected to the presintered treatment, the method further comprises the following steps:
placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves, blowing off residual water and slurry on the blank body by using an air gun, adsorbing the residual water by using dust-free cloth, and naturally air-drying at a shady and cool place. The application uses ultrasonic cleaning and burn-in method to degrease the blank, which can obviously reduce the probability of crack in blank degreasing, improve the yield of finished products and reduce the production cost.
In addition, it is notable that the higher the degreasing rate, the greater the impact on the finished product properties, the material system of the application being able to avoid the product properties from decreasing in the case when the degreasing rate is increased from 0.1 ℃/min to 10 ℃/min.
Step S4: after degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank body by using air flow, and sintering to obtain the zirconia dental floss material with the thin-wall structure.
In the embodiment of the application, the conditions of the sintering treatment are as follows: sintering at 1400-1500 deg.c for 2-4 hr.
Examples of certain embodiments of the application are given below and are not intended to limit the scope of the application.
In addition, it should be noted that the numerical values set forth in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be construed as a divisor rather than an absolute precise numerical value due to measurement errors and experimental operation problems that cannot be avoided.
Example 1
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 15 parts of trimethylolpropane triglycidyl ether, 15 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 2
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 15 parts of trimethylolpropane triglycidyl ether, 15 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
15 parts of photo-curing resin premix and 85 parts of zirconia powder are taken, stirred and then put into a ball milling tank, 10mm and 5mm zirconia ball milling beads are added, and the ball milling beads are large: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 3
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 15 parts of trimethylolpropane triglycidyl ether, 15 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 10 parts of photo-curing resin premix and 90 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 4
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 15 parts of trimethylolpropane triglycidyl ether, 15 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 25 parts of photo-curing resin premix and 75 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 5
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 15 parts of trimethylolpropane triglycidyl ether, 15 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 6
40 parts of epoxy acrylate, 20 parts of hydroxyethyl acrylate, 20 parts of trimethylolpropane triglycidyl ether, 20 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 7
40 parts of epoxy acrylate, 25 parts of hydroxyethyl acrylate, 25 parts of trimethylolpropane triglycidyl ether, 25 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 8
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 25 parts of trimethylolpropane triglycidyl ether, 20 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 0.2 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
Example 9
40 parts of epoxy acrylate, 15 parts of hydroxyethyl acrylate, 20 parts of trimethylolpropane triglycidyl ether, 25 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent SN-9228, 4 parts of liquid paraffin and 1 part of defoaming agent B-0847 are placed into a beaker, and the mixture is stirred for 24 hours and then placed into a vacuum stirring tank for vacuum stirring and defoaming treatment, so that the photo-curing resin premix is obtained.
Taking 20 parts of photo-curing resin premix and 80 parts of zirconia powder, stirring, putting into a ball milling tank, adding 10mm and 5mm zirconia ball milling beads, and carrying out large ball milling: ball milling beads: the mass ratio of the sizing agent is 1:2:2; ball milling for 24 hours, and taking out to obtain the DLP photo-curing slurry.
The micron-sized zirconia powder is heated to 1200 ℃ and calcined for 4 hours, and is ground after the calcination, the powder is sieved by a 40-mesh screen, oversized particles are sieved out, the fine powder is sieved by an 80-mesh screen, and the powder remained on the 80-mesh screen is used as the zirconia powder subjected to presintered treatment.
Pouring the DLP photo-curing slurry into a DLP photo-curing machine, and printing according to a model to obtain a dental floss blank; placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves for 10min, blowing off residual water and slurry on the blank body with an air gun, adsorbing the residual water with dust-free cloth, and naturally air-drying at a shady and cool place; putting the dental floss blank into a corundum ark, paving zirconia powder subjected to presintering treatment in the corundum ark, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; placing the tooth surface of the tooth socket blank upwards into a corundum ark, and filling all the concave surfaces on the inner side of the tooth socket with zirconia powder subjected to presintered treatment; and (3) placing the corundum ark into a degreasing furnace, degreasing at 100-500 ℃ at a heating rate of 10 ℃/min, and heating to 1000 ℃ after degreasing, and preserving heat for 2 hours.
After degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank by using air flow, and then placing the zirconia powder into a muffle furnace to sinter for 2 hours at 1450 ℃ to obtain the zirconia dental floss material with the thin-wall structure.
The zirconia dental covers of examples 1 to 9 and the commercially available zirconia dental porcelain were tested for hardness and flexural strength according to national standards, and the test results are shown in table 1.
TABLE 1
In summary, as can be seen from table 1, the thin-wall zirconia dental floss material for DLP provided by the embodiment of the application can obtain hardness similar to that of standard zirconia. In addition, it was found from the comparison of examples 1 to 4 that the improvement in the solid phase content of zirconia powder has less influence on hardness due to the bottom-up forming mode which is unique to DLP, but has a large influence on flexural strength. This is because an excessively high solid phase content increases stress upon pulling, affecting the bonding effect between layers, and thus the bending strength. It should be noted that the interlayer bonding force of the DLP is the combined action of various factors such as curing time, curing thickness, resin formula, equipment parameters and the like, and the effect of 80wt% of solid phase content is better on the premise of controlling variables in the experiment. In addition, according to the comparison of examples 1 and 5, it can be demonstrated that the material system of the present experiment can avoid the degradation of the product performance in the case when the degreasing rate is increased from 0.2 ℃/min to 10 ℃/min.
The foregoing description of the preferred embodiments of the application is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the application.

Claims (10)

1. The preparation method of the zirconia dental floss material with the thin-wall structure is characterized by comprising the following steps:
mixing 30-50 parts of epoxy acrylate, 15-25 parts of hydroxyethyl acrylate, 15-25 parts of trimethylolpropane triglycidyl ether, 15-25 parts of 1, 6-hexanediol diacrylate, 0.1-0.5 part of diphenyl- (2, 4, 6-trimethyl benzoyl) phosphorus oxide, 2-8 parts of dispersing agent, 2-6 parts of liquid paraffin and 0.5-1.5 parts of defoamer in a vacuum stirring manner to obtain a photo-curing resin premix;
ball milling and mixing zirconia powder and the photo-curing resin premix, and stirring in vacuum to obtain DLP photo-curing slurry;
printing by using the DLP photo-curing slurry to obtain a dental socket blank, filling all the concave surfaces on the inner side of the dental socket blank with pre-sintered zirconia powder, degreasing at 100-500 ℃ at a heating rate of 0.1-10 ℃/min, heating to 1000-1200 ℃ after degreasing, and preserving heat for 1-3 hours;
after degreasing, blowing off the zirconia powder subjected to presintered treatment on the blank body by using air flow, and sintering to obtain the zirconia dental floss material with the thin-wall structure.
2. The method for preparing a zirconia dental floss material with a thin wall structure according to claim 1, wherein the conditions of the sintering treatment are as follows: sintering at 1400-1500 deg.c for 2-4 hr.
3. The method for producing a thin-walled structured zirconia dental floss material according to claim 1, wherein the zirconia powder is a nearly spherical powder having an average particle diameter of 300 to 400 nm.
4. The method for preparing the thin-wall structured zirconia dental floss material according to claim 1, wherein the inner concave surface of the dental floss blank body is fully filled with zirconia powder subjected to presintered treatment, specifically:
placing the dental floss blank into a corundum square boat, paving zirconia powder subjected to presintered treatment in the corundum square boat, wherein the thickness of the zirconia powder is larger than the maximum depth of the inner side of the dental floss blank; and (3) placing the tooth surface of the dental floss blank upwards into a corundum ark, so that the concave surface on the inner side of the dental floss is fully filled with the zirconia powder subjected to presintered treatment.
5. The method for preparing a zirconia dental floss material with a thin-wall structure according to claim 1, wherein the zirconia powder subjected to the presintered treatment is:
heating micrometer zirconia powder to 1100-1300 ℃ and calcining for 3-5h, grinding after calcining, sieving with a 40-50 mesh screen, sieving to remove oversized particles, sieving with a 80-90 mesh screen to remove fine powder, and obtaining the powder on the 80-90 mesh screen, namely the zirconia powder after presintered treatment.
6. The method for preparing a thin-wall structured zirconia dental floss material according to claim 1, wherein before filling the inner concave surface of the dental floss blank with the zirconia powder subjected to the presintered treatment, the method further comprises:
placing the dental floss blank body into a beaker, using water as a medium, cleaning with ultrasonic waves, blowing off residual water and slurry on the blank body by using an air gun, adsorbing the residual water by using dust-free cloth, and naturally air-drying at a shady and cool place.
7. The method for preparing a zirconia dental floss material with a thin-wall structure according to claim 1, wherein the dispersing agent is one or more of EFKA4703, SN-9228, solsperse AC7570 and Solsperse 41000.
8. The method for preparing the zirconia dental floss material with the thin-wall structure according to claim 1, wherein the antifoaming agent is one or more of B-0846, B-0847 and B-0848 in any proportion.
9. The method for preparing the zirconia dental floss material with the thin-wall structure according to claim 1, wherein the photo-curing resin premix comprises the following raw materials in parts by weight:
40 parts of epoxy acrylate, 20 parts of hydroxyethyl acrylate, 20 parts of trimethylolpropane triglycidyl ether, 20 parts of 1, 6-hexanediol diacrylate, 0.3 part of diphenyl- (2, 4, 6-trimethylbenzoyl) phosphorus oxide, 6 parts of dispersing agent, 4 parts of liquid paraffin and 1 part of defoamer.
10. The zirconia dental floss material with the thin wall structure is characterized in that the zirconia dental floss material with the thin wall structure is prepared by the preparation method of the zirconia dental floss material with the thin wall structure according to any one of claims 1 to 9.
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