Granulation raw material, presintered body, zirconia porcelain block, fast firing production method and application

Abstract

The invention provides a granulation raw material, a pre-sintered body, a zirconia porcelain block, a fast firing production method and application. The fast firing production method comprises the following steps: S1, providing a first zirconium oxide material and a second zirconium oxide material; s2, compounding the first zirconium oxide material and the second zirconium oxide material, and granulating together with an auxiliary material to obtain a granulation raw material; s3, obtaining a green body based on the granulation raw materials; s4, carrying out pre-sintering treatment on the green body to obtain a pre-sintered body; and S5, machining the pre-sintered body, and then carrying out fast firing treatment to obtain the zirconium oxide porcelain block. On the basis of compounding of granulation raw materials, the overall performance of the zirconia ceramic block can be improved while a pre-sintered body can be rapidly sintered.

Description

Technical Field

[0001] This invention belongs to the field of dental ceramics technology, and particularly relates to a granulated raw material, a pre-fired body, a zirconia ceramic block, a rapid firing production method, and its application. Background Technology

[0002] Zirconia ceramic blocks are a high-performance ceramic material primarily made of zirconia powder. Pure zirconia ceramic blocks are white solids, but they appear gray or pale yellow when containing impurities. By adding colorants, they can also display various other colors. Zirconia ceramic blocks are suitable for functional restorations after tooth loss, cosmetic dentistry, and restorations of functionally missing teeth. Their high strength, high toughness, corrosion resistance, and good biocompatibility make them an ideal material in the field of dental restoration.

[0003] Chinese invention patent application CN103396118A discloses a method for firing ultrafine-grained zirconia ceramics. The method uses commercially available 3Y-TZP nanopowder as raw material, which is spray-granulated and molded into green bodies. The green bodies are then placed in a sintering furnace and heated to 550–600°C at a rate of 5°C / min, held for 1–2 hours, and degreased. The furnace temperature is then rapidly increased to 1300–1400°C at a rate of 400–500°C / min, held for 1–3 minutes, and then rapidly decreased to 1150–1200°C at a rate of 150–200°C / min, held for 10–20 hours. Finally, the furnace is cooled to room temperature to obtain zirconia ceramics.

[0004] While the aforementioned patent applications reduce the time the green body spends in the high-temperature zone by increasing the heating and cooling rates during sintering, industrially, pre-sintering is typically performed first, followed by machining according to tooth profile requirements and then secondary sintering. If complete sintering is performed from the outset, it hinders subsequent machining, and if pre-sintering is not performed before shipment, the product is difficult to market. The aforementioned patent applications, which only involve a single overall sintering, are not suitable for industrial applications and cannot meet the requirement of rapid sintering of the pre-sintered body after machining. Furthermore, the aforementioned patent applications do not address improvements in granulation materials that would enable rapid sintering of the pre-sintered body while simultaneously enhancing the overall performance of the zirconia ceramic block.

[0005] In view of this, it is necessary to provide a granulated raw material, a pre-fired body, a zirconia ceramic block, a rapid firing production method and its application, in order to solve or at least alleviate the technical problem of how to improve the overall performance of the zirconia ceramic block while rapidly sintering the pre-fired body based on the improvement of the granulated raw material. Summary of the Invention

[0006] The main objective of this invention is to provide a granulated raw material, a pre-fired body, a zirconia ceramic block, a rapid firing production method, and its application, aiming to solve or at least alleviate the technical problem of how to improve the performance of the zirconia ceramic block while rapidly sintering the pre-fired body based on improvements in the granulated raw material.

[0007] To achieve the above objectives, the present invention provides a rapid firing production method for zirconia ceramic blocks, comprising the following steps:

[0008] S1 provides a first zirconium oxide material and a second zirconium oxide material;

[0009] By mass percentage, the first zirconium oxide material comprises 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO;

[0010] The second zirconium oxide material comprises 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO;

[0011] S2, the first zirconium oxide material and the second zirconium oxide material are compounded at a mass ratio of 8:0.5-5, and granulated together with auxiliary materials to obtain granulated raw materials;

[0012] S3, a green body is obtained based on the granulated raw material;

[0013] S4, pre-fire the blank to obtain a pre-fired body;

[0014] S5, the pre-fired body is mechanically processed and then subjected to rapid firing to obtain a zirconia ceramic block;

[0015] The rapid heating process includes: raising the temperature to 950-1050℃ at 200-500℃ / min, then raising it to 1540-1560℃ at 40-100℃ / min, and holding it for 10-20 minutes; after holding, lowering the temperature to 850-950℃ at 40-100℃ / min.

[0016] Furthermore, the auxiliary materials include organic polymer binders, plasticizers, and dispersants; among the auxiliary materials, the organic polymer binder includes polyvinyl alcohol, the plasticizer includes polyethylene glycol, and the dispersant includes sodium polyacrylate.

[0017] Furthermore, the mass ratio of the auxiliary material to the zirconium oxide raw material is 0.1:9-11, and the zirconium oxide raw material is the sum of the first zirconium oxide material and the second zirconium oxide material;

[0018] In the auxiliary materials, the mass ratio of organic polymer binder, plasticizer, and dispersant is 0.8-1.2:0.8-1.2:0.08-0.12.

[0019] Further, in step S3, the process of obtaining the green body based on the granulated raw material includes: pressing the granulated raw material into shape, and then cold isostatic pressing to obtain the green body; the pressing pressure is 12-18 MPa and the time is 25-35 s; the cold isostatic pressing pressure is 200-240 MPa and the time is 50-70 s.

[0020] Furthermore, the pre-firing process includes: holding the blank at 250-350°C for at least 50 minutes, and then holding it at 950-1050°C for at least 50 minutes.

[0021] The present invention also provides a zirconia ceramic block, which is prepared by any of the rapid firing production methods described above.

[0022] The present invention also provides a granulation raw material for zirconia ceramic blocks, the granulation raw material comprising a first zirconia material and a second zirconia material; the mass ratio of the first zirconia material to the second zirconia material is 8:0.5-5;

[0023] By mass percentage, the first zirconium oxide material comprises 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO;

[0024] The second zirconium oxide material includes 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO.

[0025] The present invention also provides the application of any of the granulated raw materials described above in the preparation of pre-fired bodies or in the preparation of zirconia ceramic blocks.

[0026] The present invention also provides a pre-fired body of a zirconia ceramic block, wherein the granulation raw material for preparing the pre-fired body includes any of the granulation raw materials described above.

[0027] The present invention also provides a rapid firing production method based on a pre-fired body, comprising: mechanically processing the pre-fired body as described above and then subjecting it to rapid firing to obtain a zirconia ceramic block;

[0028] The rapid heating process includes: raising the temperature to 950-1050℃ at 200-500℃ / min, then raising it to 1540-1560℃ at 40-100℃ / min, and holding it for 10-20 minutes; after holding, lowering the temperature to 850-950℃ at 40-100℃ / min.

[0029] Compared with the prior art, the present invention has at least the following advantages:

[0030] This invention, based on the compounding of granulated raw materials, improves the overall performance of zirconia ceramic blocks while enabling rapid sintering of the pre-fired body. Specifically, this invention aims to simultaneously address the issues of rapid sintering and the overall performance of zirconia ceramic blocks; however, taking the first zirconia material as an example, when used alone with conventional secondary sintering methods, the secondary sintering time is long, and the overall performance needs further improvement, mainly in terms of Vickers hardness, light transmittance, flexural strength, and fracture toughness.

[0031] To achieve rapid sintering of the pre-sintered body after machining, this invention adjusts the secondary sintering method and explores the effect of rapid sintering. During rapid sintering, this invention increases the heating rate and the final holding temperature, and reduces the holding time. Experiments were conducted separately using the first zirconium oxide material and the second zirconium oxide material, but the overall performance still needs further improvement.

[0032] Unexpectedly, when using both the first and second zirconia materials as raw materials for zirconia and employing a rapid sintering method for secondary sintering, compared to conventional sintering of a single material, the Vickers hardness, light transmittance, flexural strength, and fracture toughness of the zirconia block were simultaneously guaranteed, with a shorter sintering time and higher industrialization value. It is also worth noting that, compared to experimental conditions that only reduced the heating rate, the combined use of the first and second zirconia materials did not significantly reduce the overall performance of the zirconia block with rapid heating, ensuring that this invention can obtain excellent products with a higher heating rate and a shorter secondary sintering time. Attached Figure Description

[0033] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on the structures shown in these drawings without creative effort.

[0034] Figure 1 This is a physical image of the zirconia ceramic block in the shape of a porcelain piece in Embodiment 1 of the present invention.

[0035] The realization of the objective, functional characteristics and advantages of the present invention will be further explained in conjunction with the embodiments and with reference to the accompanying drawings. Detailed Implementation

[0036] 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 a part of the embodiments of the present invention, and not all of them. 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.

[0037] Furthermore, the technical solutions of the various embodiments of the present invention can be combined with each other, but only if they are based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.

[0038] When numerical ranges are given in the embodiments, it should be understood that, unless otherwise stated in this invention, both endpoints of each numerical range and any value between the two endpoints may be selected. Unless otherwise defined, all technical and scientific terms used in this invention, as well as the prior art known to those skilled in the art and the description of this invention, may be implemented using any prior art methods, devices, and materials similar to or equivalent to those described, used, or made of materials in the embodiments of this invention; the same detection methods are used to monitor various indicators in all cases of this invention. In the embodiments and comparative examples of this invention, although some comparative examples do not involve rapid burning processes, for ease of reference and comparison, all embodiments and comparative examples maintain consistency in the description of rapid burning treatment, with the specific experimental process and parameters as the standard.

[0039] This invention provides a rapid firing method for producing zirconia ceramic blocks, comprising the following steps:

[0040] S1 provides a first zirconium oxide material and a second zirconium oxide material.

[0041] By mass percentage, the first zirconium oxide material comprises 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO.

[0042] The second zirconium oxide material comprises, by mass percentage, 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO.

[0043] Furthermore, by mass percentage, the first zirconium oxide material comprises 92-92.5 parts ZrO2, 5.0-5.2 parts Y2O3, 1.9-2.0 parts HfO2, 0.2-0.3 parts Al2O3, 0.15-0.2 parts MoO3, 0.15-0.2 parts SC2O3, and 0.05-0.06 parts ZnO.

[0044] The second zirconium oxide material comprises, by mass percentage, 89-91 parts ZrO2, 7-8 parts Y2O3, 1.5-2.0 parts HfO2, 0.2-0.25 parts Al2O3, 0.1-0.15 parts TiO2, 0.15-2.0 parts SiO2, and 0.05-0.07 parts ZnO.

[0045] Specifically, by mass percentage, the first zirconium oxide material consists of 92.285 parts of ZrO2, 5.093 parts of Y2O3, 1.983 parts of HfO2, 0.240 parts of Al2O3, 0.176 parts of MoO3, 0.169 parts of SC2O3, and 0.054 parts of ZnO.

[0046] The second zirconium oxide material, by mass percentage, consists of 90.012 parts ZrO2, 7.60 parts Y2O3, 1.783 parts HfO2, 0.220 parts Al2O3, 0.136 parts TiO2, 0.189 parts SiO2, and 0.06 parts ZnO.

[0047] It should be noted that the first zirconium oxide material and the second zirconium oxide material are key components of this invention. Only by combining the first zirconium oxide material and the second zirconium oxide material can the pre-sintered body have excellent overall performance after rapid sintering; specifically, in terms of Vickers hardness, light transmittance, flexural strength, and fracture toughness.

[0048] S2, the first zirconium oxide material and the second zirconium oxide material are mixed at a mass ratio of 8:0.5-5, and granulated together with auxiliary materials to obtain granulated raw materials.

[0049] Further, the first zirconium oxide material and the second zirconium oxide material are compounded at a mass ratio of 8:1-3, and granulated together with auxiliary materials to obtain granulated raw materials.

[0050] In this invention, the auxiliary materials include organic polymer binders, plasticizers, and dispersants; among the auxiliary materials, the organic polymer binder includes polyvinyl alcohol, the plasticizer includes polyethylene glycol, and the dispersant includes sodium polyacrylate.

[0051] In this invention, the mass ratio of the auxiliary material to the zirconium oxide raw material is 0.1:9-11, and the zirconium oxide raw material is the sum of the first zirconium oxide material and the second zirconium oxide material.

[0052] As an example, the mass ratio of the organic polymer binder, plasticizer, and dispersant in the auxiliary materials is 0.8-1.2:0.8-1.2:0.08-0.12.

[0053] As a specific description of the granulation process, the granulation process includes: mixing the first zirconium oxide material, the second zirconium oxide material and the auxiliary material together to obtain a mixture; and preparing the mixture into a slurry and spray granulating it.

[0054] The process of preparing the mixture into a slurry includes: mixing the mixture with water and then ball milling; the mass ratio of the mixture to water can be 8-9:1-2; the ball milling speed can be 200-500 rpm, the time can be 5-10 h, and the material-to-ball ratio can be 1:1-3.

[0055] S3, a green body is obtained based on the granulation raw material.

[0056] In this step, the process of obtaining the green body based on the granulated raw material includes: pressing the granulated raw material into shape, and then cold isostatic pressing to obtain the green body; as an explanation of the parameters, the pressure used for pressing is 12-18MPA and the duration is 25-35s; the pressure used for cold isostatic pressing is 200-240MPA and the duration is 50-70s.

[0057] S4, the blank is pre-fired to obtain a pre-fired body.

[0058] In this invention, the pre-sintering treatment is a single sintering process; the pre-sintering treatment process includes: holding the green body at 250-350°C for at least 50 min (moreover, 50-70 min), and then holding it at 950-1050°C for at least 50 min (moreover, 50-70 min).

[0059] As a further explanation of the pre-firing treatment, the pre-firing treatment also includes: heating at 1-3°C / min before holding at 250-350°C for at least 50 min (moreover, 50-70 min); and heating at 4-6°C / min before holding at 950-1050°C for at least 50 min (moreover, 50-70 min).

[0060] Specifically, the pre-firing process includes: raising the temperature from room temperature to 250-350°C at a heating rate of 1-3°C / min and holding it at that temperature for at least 50 min (moreover, 50-70 min); then raising the temperature to 950-1050°C at a heating rate of 4-6°C / min and holding it at that temperature for at least 50 min (moreover, 50-70 min); and finally allowing it to cool naturally.

[0061] S5, the pre-fired body is mechanically processed and then subjected to rapid firing to obtain a zirconia ceramic block.

[0062] In this invention, the rapid sintering treatment is a secondary sintering process; the rapid sintering treatment includes: raising the temperature from room temperature to 950-1050℃ at a rate of 200-500℃ / min (or 200-300℃ / min), then raising it to 1540-1560℃ at a rate of 40-100℃ / min (or 40-60℃ / min), holding it at that temperature for 10-20 min (or 14-20 min, 15-20 min, or 13-17 min); after holding at that temperature, lowering the temperature to 850-950℃ at a rate of 40-100℃ / min (or 40-60℃ / min), and finally allowing it to cool naturally.

[0063] As further explained, the rapid heating process includes: raising the temperature from room temperature to 950-1050℃ at a rate of 200-300℃ / min, then raising it to 1540-1560℃ at a rate of 40-60℃ / min, and holding it at that temperature for 13-17 minutes; after holding the temperature, lowering it to 850-950℃ at a rate of 40-60℃ / min, and finally allowing it to cool naturally.

[0064] In this invention, compared to conventional secondary sintering, by increasing the heating rate, the final sintering temperature, and reducing the holding time, secondary sintering can be completed quickly, thereby obtaining the final product rapidly after machining. It should be emphasized that not all raw materials are suitable for the rapid sintering method of this application. When only the first zirconium oxide material or only the second zirconium oxide material is used, the rapid sintering method cannot obtain the final product required by this invention.

[0065] The present invention also provides a zirconia ceramic block, which is prepared by any of the rapid firing production methods described above.

[0066] The present invention also provides a granulation raw material for zirconia ceramic blocks, the granulation raw material comprising a first zirconia material and a second zirconia material; the mass ratio of the first zirconia material to the second zirconia material is 8:0.5-5 (further 8:1-3); the granulation raw material may also include the auxiliary materials, and the proportion relationship may remain consistent with the foregoing.

[0067] In this invention, the first zirconium oxide material comprises, by mass percentage, 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO.

[0068] The second zirconium oxide material comprises, by mass percentage, 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO.

[0069] Furthermore, by mass percentage, the first zirconium oxide material comprises 92-92.5 parts ZrO2, 5.0-5.2 parts Y2O3, 1.9-2.0 parts HfO2, 0.2-0.3 parts Al2O3, 0.15-0.2 parts MoO3, 0.15-0.2 parts SC2O3, and 0.05-0.06 parts ZnO.

[0070] The second zirconium oxide material comprises, by mass percentage, 89-91 parts ZrO2, 7-8 parts Y2O3, 1.5-2.0 parts HfO2, 0.2-0.25 parts Al2O3, 0.1-0.15 parts TiO2, 0.15-2.0 parts SiO2, and 0.05-0.07 parts ZnO.

[0071] The present invention also provides the application of any of the granulated raw materials described above in the preparation of pre-fired bodies or in the preparation of zirconia ceramic blocks.

[0072] The present invention also provides a pre-fired body of a zirconia ceramic block, wherein the granulation raw material for preparing the pre-fired body includes any of the granulation raw materials described above.

[0073] Specifically, the preparation process of the pre-fired body is the same as the acquisition process of the pre-fired body in step S4 above; that is, the preparation process of the pre-fired body includes steps S1 to S4 above.

[0074] The present invention also provides a rapid firing production method based on a pre-fired body, comprising: mechanically processing the pre-fired body and then subjecting it to rapid firing treatment to obtain zirconia ceramic blocks; the rapid firing treatment comprising: raising the temperature to 950-1050℃ at 200-500℃ / min (or 200-300℃ / min), then raising it to 1540-1560℃ at 40-100℃ / min (or 40-60℃ / min), holding it at that temperature for 10-20 min (or 14-20 min, 15-20 min, or 13-17 min); after the holding period, lowering the temperature to 850-950℃ at 40-100℃ / min (or 40-60℃ / min), and finally allowing it to cool naturally.

[0075] As further explained, the rapid heating process includes: raising the temperature to 950-1050℃ at 200-300℃ / min, then raising it to 1540-1560℃ at 40-60℃ / min, and holding it for 13-17 minutes; after holding, lowering the temperature to 850-950℃ at 40-60℃ / min, and finally allowing it to cool naturally.

[0076] Compared to pre-sintered bodies obtained from other granulated raw materials, this invention, based on a specific pre-sintered body, after mechanical processing, can quickly obtain a superior final product under high heating rate, high sintering temperature, and short sintering time. This not only significantly reduces sintering time and avoids long waiting times but also ensures product performance.

[0077] The following are specific examples of the present invention:

[0078] Example 1

[0079] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0080] S1 provides a first zirconium oxide material and a second zirconium oxide material.

[0081] By mass percentage, the first zirconium oxide material consists of 92.285 parts ZrO2, 5.093 parts Y2O3, 1.983 parts HfO2, 0.240 parts Al2O3, 0.176 parts MoO3, 0.169 parts SC2O3, and 0.054 parts ZnO.

[0082] By mass percentage, the second zirconium oxide material consists of 90.012 parts ZrO2, 7.60 parts Y2O3, 1.783 parts HfO2, 0.220 parts Al2O3, 0.136 parts TiO2, 0.189 parts SiO2, and 0.06 parts ZnO.

[0083] S2, the first zirconium oxide material, the second zirconium oxide material, and auxiliary materials are mixed together to obtain a mixture; the mixture is prepared into a slurry, thoroughly mixed, and spray-granulated to obtain a granulation raw material.

[0084] In this embodiment, the mass ratio of the first zirconium oxide material to the second zirconium oxide material is 8:2.

[0085] In this embodiment, the mass ratio of auxiliary materials to zirconium oxide raw materials is 0.1:9.9.

[0086] In this embodiment, the zirconium oxide raw material is the sum of the first zirconium oxide material and the second zirconium oxide material.

[0087] In this embodiment, the auxiliary materials consist of an organic polymer binder, a plasticizer, and a dispersant in a mass ratio of 1:1:0.1; among the auxiliary materials, the organic polymer binder is PVA (polyvinyl alcohol), the plasticizer is PEG (polyethylene glycol), and the dispersant is sodium polyacrylate.

[0088] In this embodiment, the process of preparing the mixture into a slurry is as follows: the mixture and water are mixed at a mass ratio of 8.5:1.5 and then ball-milled; the ball milling speed is 365 rpm, the time is 7 hours, and the material-to-ball ratio is 1:2.

[0089] S3, using a powder molding machine to press the granulated raw material into a disc shape, and then cold isostatically press to obtain the green body.

[0090] In this embodiment, the pressure used for compression molding is 15 MPa and the duration is 30 s; the pressure used for cold isostatic pressing is 220 MPa and the duration is 60 s.

[0091] S4. The green body is pre-fired to obtain a pre-fired body.

[0092] In this embodiment, the pre-firing process is as follows: the temperature is increased from room temperature to 300°C at a heating rate of 2°C / min and held for 60 min; then the temperature is increased to 1000°C at a heating rate of 5°C / min and held for 60 min; finally, the temperature is allowed to cool naturally.

[0093] S5, the pre-fired body is cut (cut according to test requirements, and simultaneously cut into zirconia-shaped blocks), and then subjected to rapid firing to obtain zirconia blocks; see [link to zirconia block description] for zirconia blocks in zirconia shape. Figure 1 As shown.

[0094] In this embodiment, the rapid heating process is as follows: the temperature is increased from room temperature to 1000°C at a heating rate of 250°C / min, then increased to 1550°C at a heating rate of 50°C / min, and held for 15 minutes; after the holding period, the temperature is reduced to 900°C at a cooling rate of 50°C / min, and finally cooled naturally.

[0095] 2. Test Results:

[0096] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1360 HV (5KG).

[0097] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 57%.

[0098] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 1000 MPa.

[0099] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 8.5G.

[0100] Comparative Example 1

[0101] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0102] Compared to Example 1, this comparative example omits the use of the first zirconium oxide material and uses only the second zirconium oxide material directly as the zirconium oxide raw material, while keeping other conditions unchanged.

[0103] 2. Test Results:

[0104] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1260 HV (5KG).

[0105] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 50%.

[0106] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 800 MPa.

[0107] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 6.5G.

[0108] Comparative Example 2

[0109] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0110] Compared to Example 1, this comparative example omits the use of the second zirconia material and uses only the first zirconia material directly as the zirconia raw material, while keeping other conditions unchanged.

[0111] 2. Test Results:

[0112] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1280 HV (5KG).

[0113] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 45%.

[0114] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 950 MPa.

[0115] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 7.3G.

[0116] Comparative Example 3

[0117] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0118] Compared to Example 1, this comparative example only adjusts the rapid cooking process, while keeping other conditions unchanged.

[0119] In this comparative example, the rapid heating process is as follows: the temperature is increased from room temperature to 1000℃ at a heating rate of 100℃ / min, then increased to 1500℃ at a heating rate of 20℃ / min, and held for 15min; after the holding period, the temperature is reduced to 900℃ at a cooling rate of 50℃ / min, and finally cooled naturally.

[0120] 2. Test Results:

[0121] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1000 HV (5KG).

[0122] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 45%.

[0123] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 900 MPa.

[0124] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 4.5G.

[0125] Comparative Example 4

[0126] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0127] Compared to Example 1, this comparative example only adjusts the rapid cooking process, while keeping other conditions unchanged.

[0128] In this comparative example, the rapid heating process is as follows: the temperature is increased from room temperature to 1000℃ at a heating rate of 100℃ / min, then increased to 1550℃ at a heating rate of 20℃ / min, and held for 15 minutes; after the holding period, the temperature is reduced to 900℃ at a cooling rate of 50℃ / min, and finally cooled naturally.

[0129] 2. Test Results:

[0130] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1330 HV (5KG).

[0131] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 56%.

[0132] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 1020 MPa.

[0133] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 8.6G.

[0134] Comparative Example 5

[0135] 1. A method for producing zirconia ceramic blocks, comprising the following steps:

[0136] Compared to Example 1, this comparative example only uses the first zirconium oxide material as the zirconium oxide raw material and adjusts the rapid calcination process, while keeping other conditions unchanged.

[0137] In this comparative example, the rapid heating process was as follows: the temperature was increased from room temperature to 1000℃ at a heating rate of 10℃ / min, then increased to 1500℃ at a heating rate of 20℃ / min, and held for 120min; after the holding period, the temperature was reduced to 900℃ at a cooling rate of 50℃ / min, and finally cooled naturally.

[0138] 2. Test Results:

[0139] The hardness of the zirconia ceramic block was tested according to GB / T 16534-2009 standard, and its Vickers hardness was 1200 HV (5KG).

[0140] The light transmittance of the zirconia ceramic block was tested according to GB / T 2410-2008 standard, and its light transmittance was 45%.

[0141] The flexural strength of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its flexural strength was 950 MPa.

[0142] The fracture toughness of the zirconia ceramic block was tested according to ISO 6872:2015 standard, and its fracture toughness was 5.5G.

[0143] The above technical solutions of the present invention are merely preferred embodiments of the present invention and do not limit the patent scope of the present invention. All equivalent structural transformations made under the technical concept of the present invention using the contents of the present invention specification and drawings, or direct / indirect applications in other related technical fields, are included in the patent protection scope of the present invention.

Claims

1. A method for rapid firing production of zirconia ceramic blocks, characterized in that, Including the following steps: S1 provides a first zirconium oxide material and a second zirconium oxide material; By mass percentage, the first zirconium oxide material comprises 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO; The second zirconium oxide material comprises 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO; S2, the first zirconium oxide material and the second zirconium oxide material are compounded at a mass ratio of 8:0.5-5, and granulated together with auxiliary materials to obtain granulated raw materials; S3, a green body is obtained based on the granulated raw material; S4, pre-fire the blank to obtain a pre-fired body; S5, the pre-fired body is mechanically processed and then subjected to rapid firing to obtain a zirconia ceramic block; The rapid heating process includes: raising the temperature to 950-1050℃ at a rate of 200-500℃ / min, then raising it to 1540-1560℃ at a rate of 40-100℃ / min, and holding it at that temperature for 10-20 minutes. After the heat preservation is completed, the temperature is reduced to 850-950℃ at a rate of 40-100℃ / min.

2. The rapid-fire production method according to claim 1, characterized in that, The auxiliary materials include organic polymer binders, plasticizers, and dispersants; among the auxiliary materials, the organic polymer binder includes polyvinyl alcohol, the plasticizer includes polyethylene glycol, and the dispersant includes sodium polyacrylate.

3. The rapid-fire production method according to claim 2, characterized in that, The mass ratio of the auxiliary material to the zirconium oxide raw material is 0.1:9-11, and the zirconium oxide raw material is the sum of the first zirconium oxide material and the second zirconium oxide material; In the auxiliary materials, the mass ratio of organic polymer binder, plasticizer, and dispersant is 0.8-1.2:0.8-1.2:0.08-0.

12.

4. The rapid-fire production method according to claim 1, characterized in that, In step S3, the process of obtaining the green body based on the granulated raw material includes: pressing the granulated raw material into shape, and then cold isostatic pressing to obtain the green body; the pressing pressure is 12-18 MPa and the time is 25-35 s; the cold isostatic pressing pressure is 200-240 MPa and the time is 50-70 s.

5. The rapid-fire production method according to claim 1, characterized in that, The pre-firing process includes: holding the blank at 250-350°C for at least 50 minutes, and then holding it at 950-1050°C for at least 50 minutes.

6. A zirconia ceramic block, characterized in that, It is prepared by the rapid calcination production method as described in any one of claims 1-5.

7. A granulation raw material for zirconia ceramic blocks, characterized in that, The granulation raw materials include a first zirconium oxide material and a second zirconium oxide material; the mass ratio of the first zirconium oxide material to the second zirconium oxide material is 8:0.5-5; By mass percentage, the first zirconium oxide material comprises 91-93 parts ZrO2, 4.5-5.5 parts Y2O3, 1.5-2.5 parts HfO2, 0.2-0.3 parts Al2O3, 0.1-0.2 parts MoO3, 0.1-0.2 parts SC2O3, and 0.04-0.07 parts ZnO; The second zirconium oxide material includes 88-92 parts ZrO2, 6-9 parts Y2O3, 1-3 parts HfO2, 0.15-0.3 parts Al2O3, 0.1-0.2 parts TiO2, 0.15-2.5 parts SiO2, and 0.04-0.08 parts ZnO.

8. The use of the granulated raw material as described in claim 7 in the preparation of pre-fired bodies or in the preparation of zirconia ceramic blocks.

9. A pre-fired body of a zirconia ceramic block, characterized in that, The granulation raw material for preparing the pre-burned body includes the granulation raw material as described in claim 7.

10. A rapid firing production method based on pre-fired body, characterized in that, include: The pre-fired body as described in claim 9 is subjected to rapid firing after mechanical processing to obtain a zirconia ceramic block; The rapid heating process includes: raising the temperature to 950-1050℃ at a rate of 200-500℃ / min, then raising it to 1540-1560℃ at a rate of 40-100℃ / min, and holding it at that temperature for 10-20 minutes. After the heat preservation is completed, the temperature is reduced to 850-950℃ at a rate of 40-100℃ / min.

Images