Preparation method of occlusal plate based on force-induced luminescent material

Abstract

The application discloses a preparation method of a bite plate based on a force-induced luminescent material. It belongs to the technical field of oral bite plates and can prepare a bite plate capable of directly and real-timely converting bite force into a visible light signal through a simple process, so that the visualization and semi-quantitative detection of bite contact are realized. The preparation method of the bite plate based on the force-induced luminescent material is characterized in that the method comprises the following steps: (1) synthesizing europium / dysprosium co-doped strontium aluminate force-induced luminescent material SAOED by using a high-temperature solid-phase method, wherein the doping concentration of europium is 2%, and the doping concentration of dysprosium is 1%; (2) mixing the SAOED powder obtained in the step (1) with denture powder according to a mass ratio of 1:7, adding ethanol for dispersion and grinding; (3) adding denture water in a proportion corresponding to the denture powder to the mixture in the step (2), uniformly stirring, and then performing compression molding; and (4) performing water bath heating solidification on the compression molded material, and then performing polishing to obtain the bite plate.

Description

Technical Field

[0001] This invention relates to the field of oral occlusal plate technology, specifically a method for preparing an occlusal plate based on a mechanoluminescent material. Background Technology

[0002] In clinical dentistry, accurate assessment of occlusal contact position and pressure magnitude is crucial. Currently widely used traditional methods, such as occlusal papers, only provide qualitative or semi-qualitative information on contact point location, failing to intuitively reflect the actual magnitude and distribution gradient of occlusal force. Furthermore, the results are easily affected by operational factors, have poor repeatability, and rely heavily on the dentist's experience. While existing electronic occlusal analyzers can achieve quantitative measurement, the equipment is expensive and bulky, hindering routine adoption.

[0003] In recent years, some studies have attempted to introduce functional materials such as piezoelectric materials into occlusal examination. For example, piezoelectric materials can convert occlusal force into electrical energy, which then drives a light-emitting unit. However, such technical solutions are usually structurally complex, involving multi-stage energy conversion and circuit connections. Their core purpose is often to achieve therapeutic functions (such as antibacterial properties) rather than to provide direct, highly sensitive visualization of the occlusal contact itself. Their complex structure and energy conversion pathways also increase manufacturing costs and the reliability risks of the instruments in the oral environment.

[0004] Therefore, it is urgent to develop a method for preparing interlocking plates based on mechanoluminescent materials to solve the problems in the existing technology. Summary of the Invention

[0005] The purpose of this invention is to provide a method for preparing a bite plate based on a mechanoluminescent material, which can produce a bite plate that can directly and in real time convert bite force into a visible light signal through a simple process, thereby realizing the visualization and semi-quantitative detection of bite contact, and solving the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution: A method for preparing a mechanoluminescent interlocking plate includes the following steps: (1) Europium / dysprosium co-doped strontium aluminate mechanoluminescent material SAOED was synthesized by a high-temperature solid-state method, wherein The doping concentration is 2%. The doping concentration is 1%; By adopting the above technical solution, a chemical composition of [missing information] was obtained. : , Functional powder. This specific doping concentration ( 2%, The combination of 1% enables the material to release a high-intensity and stable visible light signal when subjected to mechanical stress, which is the basis for realizing the visualization of biting force.

[0007] (2) Mix the SAOED powder obtained in step (1) with the dental tray powder at a mass ratio of 1:7, and add ethanol for dispersion and grinding; By employing the above technical solution, inorganic mechanoluminescent powder and organic resin powder are physically mixed. Ethanol, acting as a wetting agent and dispersion medium, helps reduce the agglomeration of SAOED powder. The grinding action promotes uniform microscopic mixing of the two, laying the foundation for the subsequent formation of a homogeneous composite material. This is crucial for ensuring consistent luminescent response across all parts of the interlocking plate under stress.

[0008] (3) Add dental tray water in proportion to the dental tray powder to the mixture in step (2), stir evenly, and then press and mold it. By employing the above technical solution, the monomers in the dental tray water initiate a polymerization reaction, transforming the mixed powder from a dispersed state into a plastic, dough-like material. The compression molding step imparts a preliminary macroscopic shape and density to the material, giving it the basic form required for subsequent processing.

[0009] (4) The pressed material is heated and cured in a water bath, and then polished to obtain the interlocking plate.

[0010] By employing the above technical solution, water bath heating provides a uniform and controlled temperature environment, promoting the complete polymerization and curing of resin monomers to form a stable three-dimensional network structure that firmly embeds SAOED particles within it. The grinding and polishing process removes burrs and unevenness from the molding process, resulting in a smooth surface and rounded edges on the occlusal plate, meeting the surface requirements for medical devices that can be directly placed in the oral cavity.

[0011] As a further aspect of the present invention: in step (2), the dispersion and grinding time is 10-30 minutes.

[0012] By adopting the above technical solution, an optimized time range was established. Too short a time (<10 minutes) may result in insufficient dispersion and powder agglomeration; too long a time (>30 minutes) may cause the powder to be too fine or introduce too many impurities, or even cause the mixture to dry prematurely due to ethanol evaporation. This range balances dispersion effect and process efficiency.

[0013] As a further aspect of the present invention: in step (3), the pressing and molding is carried out in a mold, and the cavity of the mold is a full tooth row covering structure.

[0014] By employing the above-mentioned technical solution, the mold cavity restricts the material, allowing it to be directly molded into a specific structure capable of simultaneously covering all teeth in the maxilla or mandible. This ensures that the product's shape matches the patient's dental arch shape, making it a necessary physical form to achieve its clinical function (covering the entire dentition for occlusal examination).

[0015] As a further aspect of the present invention: by controlling the cavity depth of the mold, the thickness of the interlocking plate obtained in step (4) is 2-3 mm.

[0016] By adopting the above technical solution, the final thickness of the product was limited. The thickness range of 2-3mm is based on the balance between clinical needs and the mechanical properties of the material: a thickness of less than 2mm may lead to insufficient strength, easy deformation or breakage; a thickness of more than 3mm will significantly reduce the space in the oral cavity, affect wearing comfort, and may interfere with normal occlusal sensation.

[0017] As a further aspect of the present invention: in step (4), the water bath heating and curing temperature is 60-80℃ and the time is 30-90 minutes.

[0018] By adopting the above technical solution, a process parameter window for fully curing the resin is defined. Temperature and time work synergistically within this range: if the temperature is too low or the time is too short, the resin polymerization will be incomplete, resulting in low material strength and a high amount of residual monomers; if the temperature is too high or the time is too long, it may lead to resin degradation, discoloration, or the generation of internal stress. This range ensures the stability and reproducibility of the final product's performance.

[0019] As a further aspect of the present invention: in step (2), the amount of ethanol added is 10-20% of the total mass of SAOED powder and dental tray powder.

[0020] By adopting the above technical solution, the amount of dispersion medium was quantified. If the ethanol addition is less than 10%, the wetting is insufficient, resulting in poor flowability of the mixed powder and difficulty in uniform dispersion; if the addition is more than 20%, the mixture becomes too wet and sticky, which is not conducive to subsequent mixing with dental tray liquid and prolongs the waiting time for subsequent drying or evaporation. This ratio keeps the mixture in an optimal semi-dry / wet dispersion state.

[0021] As a further aspect of the present invention: in step (1), the synthesis temperature of the high-temperature solid-state method is 1300-1500℃, and the holding time is 2-4 hours.

[0022] By adopting the above technical solution, the sintering process conditions for obtaining high-performance SAOED materials were clarified. This temperature and time range ensures complete solid-state reaction of the raw materials, formation of pure-phase crystals, and... Ions are effectively reduced to luminescent centers ( This is necessary. Insufficient temperature or time will result in poor crystallinity and weak luminescence properties in the product; excessively high temperature may lead to component volatilization or phase change.

[0023] As a further aspect of the present invention: in step (4), the grinding and polishing is carried out using sandpaper or polishing cloth with progressively increasing fineness.

[0024] By employing the above-described technical solution, a progressive surface finishing method is presented. First, coarse-grained tools are used to remove obvious imperfections and excess material. Then, finer-grained tools are progressively used to eliminate scratches left from the previous step, ultimately achieving a high-gloss surface. This method is more effective than single-step polishing, resulting in a smoother surface, reducing plaque buildup, and improving patient comfort.

[0025] Compared with existing technologies, the advantages of this invention are as follows: by using a specific ratio of composite mechanoluminescent materials and resin, the occlusal plate can directly and in real-time convert occlusal force into visible light, realizing the visualization of occlusal contact. Its luminescence intensity is positively correlated with stress, allowing for semi-quantitative assessment of pressure distribution. This product is easy to operate, requires no auxiliary consumables, and provides intuitive and reproducible results. Furthermore, while possessing excellent luminescent performance, it maintains good mechanical strength, wear resistance, and biocompatibility, meeting the core requirements for clinical oral use.

[0026] Other features and advantages of the present invention will be disclosed in detail in the following detailed description and accompanying drawings. Attached Figure Description

[0027] Figure 1 This is a schematic diagram of the bite plate in an embodiment of the present invention. Detailed Implementation

[0028] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0029] Example 1: Preparation of SAOED / DBR composite interlocking plate using standard process (1) Synthesis of mechanoluminescent material SAOED: Accurately weigh strontium carbonate ( 17.73g, aluminum oxide ( 10.20g, europium oxide ( 0.35g and dysprosium oxide ( 0.19g (corresponding to stoichiometry) : (2%), (1%). The raw materials were placed in a planetary ball mill, using anhydrous ethanol as the medium and zirconia balls as the grinding balls, and milled at 300 rpm for 6 hours. The mixed slurry was dried in an oven at 80°C for 12 hours and then passed through a 200-mesh sieve. The precursor powder was placed in an alumina crucible and then placed in a tube furnace. A flowing reducing atmosphere (95%) was introduced. +5% The temperature was increased to 1450℃ at a flow rate of 200 mL / min and held for 3.5 hours, then decreased to 200℃ at a flow rate of 2℃ / min and cooled in the furnace. The sintered block was ground and passed through a 400-mesh sieve to obtain a light yellow SAOED powder.

[0030] (2) Preparation and compression molding of composite materials: Weigh 2.0g of SAOED powder obtained in step (1) and mix it with 14.0g of polymethyl methacrylate (PMMA) based denture powder in a glass mortar. Add 2.4g of anhydrous ethanol (15% of the total powder mass) and grind by hand for 20 minutes. Then add 7.0mL of denture liquid (matching the denture powder) and stir quickly until it forms a dough. Fill the dough into a silicone rubber negative mold replicated according to a standard mandibular plaster model, place it on a press and press it at 0.5MPa for 5 minutes to form a preform.

[0031] (3) Curing and post-treatment: The model containing the preform was completely immersed in a constant temperature water bath at 70±1℃ and cured for 60 minutes. After demolding, the edges were first trimmed with a technician's grinder and a crack drill, then polished under running water using 400-grit, 600-grit, and 800-grit wet sandpaper in sequence. Finally, a cloth wheel dipped in denture polishing compound was used for polishing. Using a digital micrometer, the average thickness of the final occlusal plate was measured at multiple points to be 2.4±0.1mm.

[0032] Example 2: Short-time dispersion and low-temperature curing process The difference from Example 1 is as follows: In step (2), the amount of ethanol added is 10% of the total mass of the powder (i.e., 1.6g), and the dispersion and grinding time is 10 minutes.

[0033] In step (3), the water bath curing temperature is 60℃ and the time is 90 minutes.

[0034] The remaining steps and raw materials are the same as in Example 1.

[0035] Example 3: Long-term dispersion and high-temperature curing process The difference from Example 1 is as follows: In step (2), the amount of ethanol added is 20% of the total mass of the powder (i.e., 3.2g), and the dispersion and grinding time is 30 minutes.

[0036] In step (3), the water bath curing temperature is 80℃ and the time is 30 minutes.

[0037] The remaining steps and raw materials are the same as in Example 1.

[0038] Comparative Example 1: Pure Resin Interlocking Board No SAOED powder is added. Weigh 16.0g of the same denture powder directly, add 8.0mL of denture water to mix, and then process it through the same pressing, curing (70℃ / 60 minutes) and polishing process to make pure DBR occlusal plates.

[0039] Experimental testing and data analysis The samples prepared above were systematically tested, and the results are as follows: 1. Methluminescence performance test Test method: A dynamic compressive load (frequency 2Hz, peak force 5N, 10N, 15N) was applied to the sample (10mm×10mm×2mm specimen) using a universal testing machine. Simultaneously, a darkroom system equipped with photomultiplier tubes was used to synchronously acquire the luminous signal. The output voltage (V) was amplified and recorded as a quantitative indicator of luminous intensity.

[0040] Experimental results: Sensitivity and Linearity: Within the load range of 5-15 N, all sample examples exhibited mechanoluminescence response. Taking the sample of Example 1 as an example, the fitted curve of its output voltage (V) versus applied pressure (N) was y=0.32x+0.05, with a linear correlation coefficient of... =0.992, indicating a highly linear positive correlation between luminescence intensity and stress. The linear slopes for Examples 2 and 3 are 0.29 and 0.31, respectively. All are greater than 0.98.

[0041] Uniformity: Under a 10N load, the relative standard deviation (RSD) of the luminescence intensity at five different locations on the sample surface was 4.2% for Example 1, 7.8% for Example 2, and 4.5% for Example 3. This indicates that Example 1 exhibited the best dispersion uniformity.

[0042] 2. Mechanical performance testing Shore hardness (D scale): tested according to GB / T2411-2008 standard. Results: Example 1: 86.2±1.3; Example 2: 85.5±1.5; Example 3: 86.0±1.4; Comparative Example 1: 86.5±1.1. One-way ANOVA showed no significant difference between the examples and Comparative Example 1 (p>0.05).

[0043] Volumetric wear rate: A dental mastication simulation tester (SDMechatronik) was used with talc ceramic grinding balls, a load of 50 N, a frequency of 1.2 Hz, and 500,000 cycles in artificial saliva at 37°C. The wear volume was measured using a three-dimensional white light interferometer (ZygoNewView9000).

[0044] Wear volume (mm) 3Comparative Example 1: 0.152±0.012; Example 1: 0.123±0.010; Example 2: 0.130±0.011; Example 3: 0.125±0.009.

[0045] Conclusion: Compared with pure resin, the wear rate of the composite interlocking plates in Examples 1-3 was reduced by approximately 15%-19%, and the wear resistance was significantly improved (p<0.01). This invention provides a method for preparing interlocking plates based on mechanoluminescent materials, which can produce interlocking plates that can directly and in real-time convert interlocking force into visible light signals through a simple process, thereby achieving visualization and semi-quantitative detection of interlocking contact with high reliability.

[0046] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.

[0047] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A method for preparing a mechanoluminescent interlocking plate, characterized in that, Includes the following steps: (1) Europium / dysprosium co-doped strontium aluminate mechanoluminescent material SAOED was synthesized by a high-temperature solid-state method, wherein The doping concentration is 2%. The doping concentration is 1%; (2) Mix the SAOED powder obtained in step (1) with the dental tray powder at a mass ratio of 1:7, and add ethanol for dispersion and grinding; (3) Add dental tray water in proportion to the dental tray powder to the mixture in step (2), stir evenly, and then press and mold it. (4) The pressed material is heated and cured in a water bath, and then polished to obtain the interlocking plate.

2. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (2), the dispersion and grinding time is 10-30 minutes.

3. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (3), the pressing and molding is carried out in a mold, and the cavity of the mold is a full tooth row covering structure.

4. The method for preparing a mechanoluminescent interlocking plate according to claim 3, characterized in that, By controlling the cavity depth of the mold, the thickness of the interlocking plate obtained in step (4) is 2-3 mm.

5. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (4), the water bath heating and curing temperature is 60-80℃ and the time is 30-90 minutes.

6. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (2), the amount of ethanol added is 10-20% of the total mass of SAOED powder and dental tray powder.

7. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (1), the synthesis temperature of the high-temperature solid-state method is 1300-1500℃, and the holding time is 2-4 hours.

8. The method for preparing a mechanoluminescent interlocking plate according to claim 1, characterized in that, In step (4), the grinding and polishing is carried out using sandpaper or polishing cloth with progressively increasing fineness.

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