Method for manufacturing transparent alumina bracket on basis of high-solid-content and high-viscosity ceramic paste
Through the high-solid, high-viscosity ceramic paste manufacturing method, the preparation process of alumina brackets is optimized, and the problem of uneven distribution of sintering additives in the traditional method is solved, and the alumina brackets with stable product performance and high light transmittance are realized, simplifying the preparation process.
Patent Information
- Application Number
- PCT/CN2024/130359
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-01-31
- Filing Date
- 2024-11-07
- Publication Date
- 2025-08-07
AI Technical Summary
The preparation process of existing alumina brackets is complex, and the distribution of sintering additives is uneven, resulting in unstable product performance. It is difficult for traditional methods to control pores and pore sizes, affecting the correction effect.
The high-solid and high-viscosity ceramic paste manufacturing method is adopted, and the process flow is optimized to achieve uniform distribution and high light transmittance by mixing nitrate solution, photosensitive resin and α-alumina powder, adding dispersant and rheological additives.
It shortens the preparation cycle, improves product performance stability and light transmittance, simplifies the post-treatment process, avoids impurity ion residues, and improves the correction effect.
Smart Images

Figure CN2024130359_07082025_PF_FP_ABST
Abstract
Description
A method for manufacturing transparent alumina brackets based on high-solidity and high-viscosity ceramic paste Technical Field
[0001] The present invention relates to medical devices, and in particular to a method for manufacturing a transparent alumina bracket based on a high-solid and high-viscosity ceramic paste. Background Art
[0002] Brackets are a type of medical device used to fix and correct teeth. They are used to assist the archwire in applying various types of corrective forces to the teeth to achieve the purpose of orthodontic correction of teeth.
[0003] Traditional brackets are made of stainless steel, but stainless steel brackets have the following issues: 1. The color difference between the stainless steel and the teeth is too great, which can be unsightly and negatively impact the patient's mental health during treatment; 2. Some patients may suffer from metal allergies, making stainless steel brackets unsuitable for these patients; and 3. Long-term wear of stainless steel brackets can lead to metal poisoning. To address these issues, ceramic brackets have gradually emerged on the market as technology advances.
[0004] Existing ceramic brackets can be divided into two categories: white ceramic brackets and transparent ceramic brackets. Due to the difference in tooth color between patients, wearing white ceramic brackets may still cause aesthetic problems and affect patients' psychological health. In comparison, transparent ceramic brackets can be used by more patients, taking better care of patients' psychological health during orthodontic treatment, laying the foundation for achieving better orthodontic treatment results.
[0005] The most commonly used material for ceramic brackets is alumina, but alumina brackets have the following problems: 1. The preparation process is relatively complicated. The traditional wet ball milling process includes slurry preparation - ball milling - molding - degreasing - sintering, and the preparation cycle is very long; 2. In the existing process, sintering aids are added during sintering, but the sintering aids have the characteristic of easy agglomeration, so they are unevenly distributed in the product, affecting the sintering quality; 3. In order to solve the problem of uneven distribution of sintering aids, existing technologies may use impregnation solutions to assist in adding sintering aids, but this process has very high requirements on the porosity and pore size of the product, as well as the impregnation time. The process control is difficult, resulting in unstable product performance; 4. Since nitrates are insoluble or soluble in small amounts in photosensitive resins, the metal ions cannot be evenly dispersed in the resin, resulting in unstable final performance.
[0006] Summary of the Invention
[0007] Purpose of the invention: The purpose of the present invention is to provide a method for manufacturing transparent alumina brackets based on high-solid and high-viscosity ceramic paste with a short manufacturing cycle and stable product performance.
[0008] Technical solution: The method of manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste described in the present invention comprises the following steps:
[0009] The first step is to mix the nitrate solution with an organic solvent that does not participate in the photocuring reaction to obtain an organic solvent mixture;
[0010] Step 2: preparing a photosensitive resin premix, mixing the organic solvent mixture with the photosensitive resin premix to obtain a resin mixture, wherein the mass of the organic solvent that does not participate in the photocuring reaction is 5% to 20% of the mass of the resin mixture;
[0011] Step 3: Add a photoinitiator to the resin mixture obtained in the second step, and then add α-alumina powder and a dispersant with a purity greater than 99.99% in several times, and homogenize them in a homogenizer after adding the α-alumina powder and dispersant each time. After 90% by weight of the α-alumina powder and dispersant are added, place them in a ball mill and mill them to obtain a first mixture. The remaining 10% by weight of the α-alumina powder and dispersant are mixed with the first mixture and homogenized in a homogenizer to obtain a homogeneous mixture. A rheological additive is added to the homogeneous mixture to adjust its rheological properties, thereby obtaining a light-cured additive manufacturing paste. The light-cured additive manufacturing paste is placed in a vacuum machine for vacuum degassing. The solid content G of the light-cured additive manufacturing paste is ≥66 vol% (volume ratio), and the viscosity of the light-cured additive manufacturing paste at room temperature is 85000 mPa·s≤η≤90000 mPa·s;
[0012] Step 4: Place the light-curing additive manufacturing paste after vacuum degassing in the third step into the additive manufacturing equipment for light-curing forming to obtain a green body;
[0013] Step 5: placing the green body obtained in the fourth step into an ultrasonic cleaning device with a built-in cleaning solution, performing ultrasonic cleaning on the green body, and drying it under room temperature wind after cleaning to obtain a dried green body;
[0014] Step 6: Cold isostatic pressing: place the dried green body obtained after step 5 in an environment of 230 MPa to 260 MPa for 5 to 10 minutes.
[0015] Step 7: Place the cold isostatically pressed green body into a heating device for degreasing. The environment in the heating device is vacuum. The temperature in the heating device is raised from room temperature to 200°C at a heating rate of 1.8 to 2.2°C / min; the temperature is raised from 200°C to 400°C at a heating rate of 0.8 to 1.2°C / min; at 400°C, air is introduced into the heating device at a rate of 0.5 L / min, and the temperature is raised from 400°C to 1000°C at a heating rate of 2.8 to 3.2°C / min.
[0016] Step 8: Pre-sintering: The temperature in the heating device is raised from 1000°C to 1300°C at a heating rate of 2-3°C / min; the temperature is raised from 1300°C to 1600°C at a heating rate of 0.5-1°C / min (a lower heating rate from 1300°C to 1600°C is conducive to the discharge of pores. If the heating rate is too fast, the migration rate of the grain boundaries will be greater than the rate of pore discharge, eventually forming closed pores, which cannot be eliminated by subsequent high vacuum sintering or hot isostatic pressing). Keep at 1600°C for 0.5-2 hours.
[0017] Step 9: Place in sintering device for sintering.
[0018] Furthermore, the nitrate solution in the first step is a mixture of nitrate and deionized water, and the mass of the deionized water is 10% to 20% of the mass of the organic solvent that does not participate in the photocuring reaction.
[0019] Furthermore, the nitrate in the first step includes magnesium nitrate, yttrium nitrate and lanthanum nitrate, the mass of the magnesium nitrate is 0.02% of the mass of the α-alumina powder, the mass of the yttrium nitrate is 0.03% of the mass of the α-alumina powder, and the mass of the lanthanum nitrate is 0.03% of the mass of the α-alumina powder.
[0020] Furthermore, the magnesium nitrate exists in the form of Mg(NO3)2·6H2O, the yttrium nitrate exists in the form of Y(NO3)3·6H2O, and the lanthanum nitrate exists in the form of La(NO3)3·6H2O.
[0021] Furthermore, the organic solvent not participating in the photocuring reaction in the first step is one of polyethylene glycol 200, N,N-dimethylformamide, isopropyl alcohol, and N-methylpyrrolidone, or any mixture thereof.
[0022] Furthermore, the photosensitive resin premix in the second step includes a monofunctional resin and a bifunctional resin, and the mass ratio of the monofunctional resin to the bifunctional resin is 1:2 to 1:4.
[0023] Furthermore, the mass of the photoinitiator in the third step is 0.8% to 1.2% of the mass of the photosensitive resin premix in the second step.
[0024] Furthermore, the mass of the dispersant in the third step is 0.8% to 1.2% of the mass of the photosensitive resin premix in the second step.
[0025] Furthermore, in the third step, the particle size D50 of the α-alumina powder is 200 mm to 420 nm, and the specific surface area is 6 m 2 / g~10m 2 / g.
[0026] Furthermore, in the third step, the rotation speed of the ball mill is 280-300 rpm, the total ball milling time is 500-600 min, and the ball milling rhythm is forward rotation for 4-6 min, reverse rotation for 4-6 min, and rest for 1-3 min.
[0027] Furthermore, in the third step, the speed of the homogenizer is 1200 to 1800 rpm, and the homogenization time of the homogenizer is 10 to 30 seconds.
[0028] Furthermore, the cleaning solution in the fifth step includes resin monomer, isopropyl alcohol and polyethylene glycol 200, and the mass ratio of the resin monomer, isopropyl alcohol and polyethylene glycol 200 is 1:1:1.
[0029] Furthermore, the sintering device in the ninth step is a tungsten steel sintering device, and the environment inside the tungsten steel sintering device is vacuum, and the vacuum degree is less than 1×10 -3 Pa, the temperature environment in the sintering device is increased from 1600℃ to 1820℃, the heating rate is 2-3℃ / min, and the temperature is kept for 2-4 hours.
[0030] Furthermore, the sintering device in the ninth step is a hot isostatic pressing furnace, the environment in the hot isostatic pressing furnace is 200-300 MPa, the atmosphere is argon, the temperature environment in the sintering device is 1700° C., and the temperature is kept at 1700° C. for 2-3 hours.
[0031] Beneficial effects: Compared with the prior art, the present invention has the following significant advantages: 1. The organic solvent that does not participate in the photocuring reaction dilutes the resin premix, reduces the content of the photosensitive resin per unit volume, and makes the photosensitive resin more evenly distributed in the paste, with a high solid content and a short degreasing time. Therefore, the present invention can shorten the degreasing time, thereby shortening the preparation cycle; 2. Due to its high viscosity and self-supporting ability, no support needs to be added, simplifying the post-processing process; 3. Compared with the traditional wet ball milling method, the sintering aid (i.e., nitrate) in the present invention exists in the organic solvent mixture in the form of ions, and then is mixed with the photosensitive resin premix, photoinitiator, α-alumina powder and dispersant in turn, and can be more evenly distributed in the alumina matrix, thereby promoting sintering, and the light transmittance will be higher; 4. During the degreasing and sintering process, nitrate ions will be discharged from the product in a gaseous state, and no impurity ions will remain in the product. BRIEF DESCRIPTION OF THE DRAWINGS
[0032] FIG1 is a flow chart of the present invention.
[0033] FIG2 is a time trend diagram of thermal debinding and sintering according to Example 1 of the present invention.
[0034] FIG3 is a time trend diagram of thermal debinding and sintering in Example 2 of the present invention.
[0035] FIG4 is a schematic diagram showing the change in rheological properties after adding rheological additives.
[0036] FIG5 is a graph showing the relationship between viscosity and shear rate.
[0037] FIG6 is a SEM image of the surface of the product prepared according to the present invention. DETAILED DESCRIPTION
[0038] The technical solution of the present invention will be further described below with reference to the accompanying drawings.
[0039] Example 1
[0040] 1 to 3, a method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to the present invention is shown in FIG. 1 , and the steps are as follows:
[0041] The first step is to mix nitrate with deionized water to obtain a nitrate solution, wherein the mass of the deionized water is 15% of the mass of polyethylene glycol 200, the nitrate includes magnesium nitrate, yttrium nitrate and lanthanum nitrate, the mass of magnesium nitrate is 0.02% of the mass of α-alumina powder, the mass of yttrium nitrate is 0.03% of the mass of α-alumina powder, the mass of lanthanum nitrate is 0.03% of the mass of α-alumina powder, the magnesium nitrate exists in the form of Mg(NO3)2·6H2O, the yttrium nitrate exists in the form of Y(NO3)3·6H2O, and the lanthanum nitrate exists in the form of La(NO3)3·6H2O, and the nitrate solution is mixed with polyethylene glycol 200 to obtain an organic solvent mixture;
[0042] Step 2: preparing a photosensitive resin premix, the photosensitive resin premix comprising a monofunctional resin and a bifunctional resin, wherein the mass ratio of the monofunctional resin to the bifunctional resin is 1:3, mixing the organic solvent mixture with the photosensitive resin premix to obtain a resin mixture, wherein the mass of polyethylene glycol 200 is 10% of the mass of the resin mixture;
[0043] Step 3: Add photoinitiator to the resin mixture obtained in step 2. The mass of photoinitiator is 1% of the mass of the photosensitive resin premix in step 2. Then add α-alumina powder with a purity greater than 99.99% and dispersant in several batches. The particle size D50 of α-alumina powder is 200mm~420nm and the specific surface area is 6m 2 / g~10m 2 / g, each time α-alumina powder and dispersant are added, the mixture is homogenized in a homogenizer. The mass of the dispersant is 1% of the mass of the photosensitive resin premix in the second step. When 90% of the mass of the α-alumina powder and dispersant are added, the mixture is placed in a ball mill and milled to obtain a first mixture. The speed of the ball mill is 290 rpm, and the total ball milling time is 550 min. The ball milling rhythm is forward rotation for 5 min, reverse rotation for 5 min, and then rest for 2 min. The remaining 10% of the mass of the α-alumina powder and dispersant are mixed with the first mixture. and homogenizing the mixture in a homogenizer at a speed of 1500 rpm for 20 seconds to obtain a homogenous mixture. A rheological additive is added to the homogenous mixture to adjust its rheological properties, thereby obtaining a light-curing additive manufacturing paste. The light-curing additive manufacturing paste is placed in a vacuum machine for vacuum degassing. The solid content G of the light-curing additive manufacturing paste is ≥66 vol% (volume ratio), and the viscosity of the light-curing additive manufacturing paste at room temperature is 85000 mPa·s≤η≤90000 mPa·s;
[0044] Step 4: Place the light-curing additive manufacturing paste after vacuum degassing in the third step into the additive manufacturing equipment for light-curing forming to obtain a green body;
[0045] Step 5: placing the green body obtained in Step 4 into an ultrasonic cleaning device with a built-in cleaning solution, wherein the cleaning solution comprises a resin monomer, isopropyl alcohol, and polyethylene glycol 200, and the mass ratio of the resin monomer, isopropyl alcohol, and polyethylene glycol 200 is 1:1:1. The green body is ultrasonically cleaned for 5 seconds, and then dried under room temperature air to obtain a dried green body;
[0046] Step 6: Cold isostatic pressing: Place the dry green body obtained after step 5 in an environment of 250 MPa for 8 minutes:
[0047] Step 7: Place the cold isostatically pressed green body into a heating device for degreasing. The environment in the heating device is vacuum. The temperature in the heating device is raised from room temperature to 200°C at a heating rate of 2°C / min; the temperature is raised from 200°C to 400°C at a heating rate of 1°C / min; at 400°C, air is introduced into the heating device at a rate of 0.5L / min, and the temperature is raised from 400°C to 1000°C at a heating rate of 3°C / min;
[0048] Step 8: Pre-sintering: the temperature in the heating device is raised from 1000°C to 1300°C at a heating rate of 2.5°C / min; the temperature is raised from 1300°C to 1600°C at a heating rate of 0.8°C / min; and the temperature is kept at 1600°C for 1 hour;
[0049] Step 9: Place the tungsten steel in a sintering device for sintering. The environment inside the tungsten steel sintering device is vacuum, and the vacuum degree is less than 1×10 -3Pa, the temperature environment in the tungsten steel sintering device is increased from 1600℃ to 1820℃, the heating rate is 2.5℃ / min, and the temperature is kept for 2 hours.
[0050] Example 2
[0051] 1 to 3, a method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to the present invention is shown in FIG. 1 , and the steps are as follows:
[0052] The first step is to mix nitrate with deionized water to obtain a nitrate solution, wherein the mass of the deionized water is 18% of the mass of N,N-dimethylformamide, the nitrate includes magnesium nitrate, yttrium nitrate and lanthanum nitrate, the mass of magnesium nitrate is 0.02% of the mass of α-alumina powder, the mass of yttrium nitrate is 0.03% of the mass of α-alumina powder, the mass of lanthanum nitrate is 0.03% of the mass of α-alumina powder, the magnesium nitrate exists in the form of Mg(NO3)2·6H2O, the yttrium nitrate exists in the form of Y(NO3)3·6H2O, and the lanthanum nitrate exists in the form of La(NO3)3·6H2O, and the nitrate solution is mixed with N,N-dimethylformamide to obtain an organic solvent mixture;
[0053] Step 2: preparing a photosensitive resin premix, the photosensitive resin premix comprising a monofunctional resin and a bifunctional resin, wherein the mass ratio of the monofunctional resin to the bifunctional resin is 1:3.5, mixing the organic solvent mixture with the photosensitive resin premix to obtain a resin mixture, wherein the mass of N,N-dimethylformamide is 18% of the mass of the resin mixture;
[0054] Step 3: Add photoinitiator to the resin mixture obtained in step 2. The mass of photoinitiator is 0.9% of the mass of photosensitive resin premix in step 2. Then add α-alumina powder with a purity greater than 99.99% and dispersant in several batches. The particle size D50 of α-alumina powder is 200mm~420nm and the specific surface area is 6m 2 / g~10m 2 / g, each time α-alumina powder and dispersant were added, the mixture was homogenized in a homogenizer. The mass of the dispersant was 1.1% of the mass of the photosensitive resin premix in the second step. When 90% of the mass of the α-alumina powder and dispersant were added, the mixture was placed in a ball mill and milled to obtain a first mixture. The speed of the ball mill was 285 rpm, and the total milling time was 580 min. The milling rhythm was forward 5.5 min, reverse 5.5 min and then rest for 2.8 min. The remaining 10% of the mass of the α-alumina powder and dispersant was mixed with the first mixture. The mixture is mixed and homogenized in a homogenizer to obtain a homogenous mixture, the speed of the homogenizer is 1700 rpm, and the homogenization time of the homogenizer is 12 seconds; a rheological additive is added to the homogenous mixture to adjust its rheological properties, thereby obtaining a light-curing additive manufacturing paste, and the light-curing additive manufacturing paste is placed in a vacuum machine for vacuum degassing, the solid content G of the light-curing additive manufacturing paste is ≥66 vol% (volume ratio), and the viscosity of the light-curing additive manufacturing paste at room temperature is 85000 mPa·s≤η≤90000 mPa·s;
[0055] Step 4: Place the light-curing additive manufacturing paste after vacuum degassing in the third step into the additive manufacturing equipment for light-curing forming to obtain a green body;
[0056] Step 5: placing the green body obtained in Step 4 into an ultrasonic cleaning device with a built-in cleaning solution, wherein the cleaning solution comprises a resin monomer, isopropyl alcohol, and polyethylene glycol 200, and the mass ratio of the resin monomer, isopropyl alcohol, and polyethylene glycol 200 is 1:1:1. The green body is ultrasonically cleaned for 5 seconds, and then dried under room temperature air to obtain a dried green body;
[0057] Step 6: Cold isostatic pressing: Place the dry green body obtained after step 5 in an environment of 255 MPa for 5 to 10 minutes.
[0058] Step 7: Place the cold isostatically pressed green body into a heating device for degreasing. The environment in the heating device is vacuum. The temperature in the heating device is raised from room temperature to 200°C at a heating rate of 1.9°C / min; the temperature is raised from 200°C to 400°C at a heating rate of 0.9°C / min; at 400°C, air is introduced into the heating device at a rate of 0.5L / min, and the temperature is raised from 400°C to 1000°C at a heating rate of 2.9°C / min.
[0059] Step 8: Pre-sintering: the temperature in the heating device is raised from 1000°C to 1300°C at a heating rate of 2.7°C / min; the temperature is raised from 1300°C to 1600°C at a heating rate of 0.7°C / min; and the temperature is kept at 1600°C for 1.8 hours.
[0060] Step 9: Place in a hot isostatic pressing furnace for sintering. The environment in the hot isostatic pressing furnace is 270 MPa, the atmosphere is argon, the temperature environment in the hot isostatic pressing furnace is 1700°C, and keep warm at 1700°C for 2.8 hours.
[0061] The rheological properties after adding the rheological additive are shown in Figure 4, and the relationship between viscosity and shear rate is shown in Figure 5. Figures 4 and 5 show that the light-curing additive manufacturing paste in the present invention will not flow when not subjected to external force. Therefore, the light-curing additive manufacturing paste has self-supporting ability and does not require additional support. The present invention can simplify the processing after light-curing forming.
[0062] After preparation by the present invention, the SEM image of the product surface is shown in FIG6 . The surface of the product is dense, without holes, and the average grain size is about 12 microns. Its mechanical properties are better than those of products obtained by the prior art.
Claims
1. A method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste, comprising the following steps: The first step is to mix the nitrate solution with an organic solvent that does not participate in the photocuring reaction to obtain an organic solvent mixture; Step 2: preparing a photosensitive resin premix, mixing the organic solvent mixture with the photosensitive resin premix to obtain a resin mixture, wherein the mass of the organic solvent that does not participate in the photocuring reaction is 5% to 20% of the mass of the resin mixture; Step 3: Add photoinitiator to the resin mixture obtained in the second step, the mass of the photoinitiator is 0.8% to 1.2% of the mass of the photosensitive resin premix in the second step, and then add α-alumina powder with a purity greater than 99.99% and dispersant in several times, the mass of the dispersant is 0.8% to 1.2% of the mass of the photosensitive resin premix in the second step, and put it into the homogenizer for homogenization after adding the α-alumina powder and dispersant each time. When 90% of the mass of the α-alumina powder and dispersant are added, put it into the ball mill for ball milling. A first mixture is obtained, and the remaining 10% by mass of α-alumina powder and a dispersant are mixed with the first mixture and homogenized in a homogenizer to obtain a homogenous mixture. A rheological additive is added to the homogenous mixture to adjust its rheological properties, thereby obtaining a light-curable additive manufacturing paste. The light-curable additive manufacturing paste is placed in a vacuum machine for vacuum degassing, wherein the light-curable additive manufacturing paste has a solid content G of ≥ 66 vol%, and a viscosity of the light-curable additive manufacturing paste at room temperature of 85,000 mPa·s ≤ η ≤ 90,000 mPa·s; Step 4: Place the light-curing additive manufacturing paste after vacuum degassing in the third step into the additive manufacturing equipment for light-curing forming to obtain a green body; Step 5: placing the green body obtained in the fourth step into an ultrasonic cleaning device with a built-in cleaning solution, performing ultrasonic cleaning on the green body, and drying it under room temperature wind after cleaning to obtain a dried green body; Step 6: Cold isostatic pressing: place the dried green body obtained after step 5 in an environment of 230 MPa to 260 MPa for 5 to 10 minutes. Step 7: Place the cold isostatically pressed green body into a heating device for degreasing. The environment in the heating device is vacuum. The temperature in the heating device is raised from room temperature to 200°C at a heating rate of 1.8 to 2.2°C / min; the temperature is raised from 200°C to 400°C at a heating rate of 0.8 to 1.2°C / min; at 400°C, air is introduced into the heating device at a rate of 0.5 L / min, and the temperature is raised from 400°C to 1000°C at a heating rate of 2.8 to 3.2°C / min. Step 8: Pre-sintering: the temperature in the heating device is raised from 1000°C to 1300°C at a heating rate of 2-3°C / min; the temperature is raised from 1300°C to 1600°C at a heating rate of 0.5-1°C / min; the temperature is kept at 1600°C for 0.5-2 hours; Step 9: Place in sintering device for sintering.
2. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: In the first step, the nitrate solution is a mixture of nitrate and deionized water, wherein the mass of the deionized water is 10% to 20% of the mass of the organic solvent that does not participate in the photocuring reaction.
3. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The nitrate in the first step includes magnesium nitrate, yttrium nitrate and lanthanum nitrate, the mass of the magnesium nitrate is 0.02% of the mass of the α-alumina powder, the mass of the yttrium nitrate is 0.03% of the mass of the α-alumina powder, and the mass of the lanthanum nitrate is 0.03% of the mass of the α-alumina powder.
4. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The organic solvent not participating in the photocuring reaction in the first step is one of polyethylene glycol 200, N,N-dimethylformamide, isopropyl alcohol, and N-methylpyrrolidone, or any mixture thereof.
5. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The photosensitive resin premix in the second step includes a monofunctional resin and a bifunctional resin, and the mass ratio of the monofunctional resin to the bifunctional resin is 1:2 to 1:
4.
6. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: In the third step, the particle size D50 of α-alumina powder is 200mm~420nm, and the specific surface area is 6m 2 / g~10m 2 / g.
7. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The ball mill speed in the third step is 280-300 rpm, and the total ball milling time is 500-600 minutes. The ball milling rhythm is 4-6 minutes of forward rotation, 4-6 minutes of reverse rotation, and 1-3 minutes of rest. The homogenizer speed in the third step is 1200-1800 rpm, and the homogenization time is 10-30 seconds.
8. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The cleaning solution in the fifth step includes resin monomer, isopropyl alcohol and polyethylene glycol 200, and the mass ratio of the resin monomer, isopropyl alcohol and polyethylene glycol 200 is 1:1:
1.
9. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The sintering device in the ninth step is a tungsten steel sintering device, and the environment inside the tungsten steel sintering device is vacuum, and the vacuum degree is less than 1×10 -3 Pa, the temperature environment in the sintering device is increased from 1600℃ to 1820℃, the heating rate is 2-3℃ / min, and the temperature is kept for 2-4 hours.
10. The method for manufacturing a transparent alumina bracket based on a high-solidity and high-viscosity ceramic paste according to claim 1, characterized in that: The sintering device in the ninth step is a hot isostatic pressing furnace. The environment in the hot isostatic pressing furnace is 200-300 MPa, the atmosphere is argon, the temperature environment in the sintering device is 1700° C., and the temperature is kept at 1700° C. for 2-3 hours.
Citation Information
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