WO2018038295A1 - Corps fritté en zircone utilisant une cuisson réductrice et son procédé de production - Google Patents

Corps fritté en zircone utilisant une cuisson réductrice et son procédé de production Download PDF

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Publication number
WO2018038295A1
WO2018038295A1 PCT/KR2016/009484 KR2016009484W WO2018038295A1 WO 2018038295 A1 WO2018038295 A1 WO 2018038295A1 KR 2016009484 W KR2016009484 W KR 2016009484W WO 2018038295 A1 WO2018038295 A1 WO 2018038295A1
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WIPO (PCT)
Prior art keywords
sintered body
firing
reducing
color
oxide
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PCT/KR2016/009484
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English (en)
Korean (ko)
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장명철
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군산대학교 산학협력단
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Priority to PCT/KR2016/009484 priority Critical patent/WO2018038295A1/fr
Publication of WO2018038295A1 publication Critical patent/WO2018038295A1/fr

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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61C—DENTISTRY; APPARATUS OR METHODS FOR ORAL OR DENTAL HYGIENE
    • A61C13/00—Dental prostheses; Making same
    • A61C13/08—Artificial teeth; Making same
    • A61C13/083—Porcelain or ceramic teeth
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/64—Burning or sintering processes

Definitions

  • the present invention relates to a zirconia sintered body using reducing plasticity to express colors similar to natural teeth of dental zirconia blocks and a method of manufacturing the same.
  • zirconia is a well-known material, but it is the first to be used as a dental material in the dental materials industry.
  • the zirconia material's strength and chemical resistance are good enough to withstand extreme biochemical changes, including the oral cavity.
  • it is receiving great attention as a material that can be tailored according to the change in the color of the surrounding teeth due to the translucent and the individual dental environment changes that are important factors in tooth enamel.
  • the zirconia sintered body has a problem in that it is not easy to cope with light transmittance and color tone change.
  • natural teeth have a gradation (gradation) rather than a single color
  • a gradation process using glaze is required after the zirconia block is manufactured.
  • the present invention is to solve the above problems, and relates to a method for manufacturing a zirconia sintered body using a reducing firing capable of simulating the process and color and gradation similar to natural teeth.
  • the object of the present invention relates to a method for producing a dental zirconia sintered body of a color similar to that of natural teeth, comprising: a molding step of forming a zirconia molded body comprising zirconia as a main component and a redox oxide as a coloring agent; Firing the molded body in an oxidizing atmosphere; And a reducing firing step of changing the content of the reducing metal oxide by controlling at least one selected from a firing temperature, a firing time, and a reducing firing gas partial pressure in a reducing firing atmosphere for supplying the reducing firing gas to the firing furnace. do.
  • the redox oxide may include at least one of iron oxide and cobalt oxide, and the reduced metal oxide may include at least one of divalent iron oxide and divalent cobalt oxide.
  • the reducing firing gas may be at least one selected from nitrogen, argon and hydrogen.
  • the firing temperature in the reducing firing step may be in the range of 1000 to 1300 °C.
  • the chemical composition ratio of the molded body in the molding step may be a uniform whole body.
  • the molded article in the molding step may be formed of at least two layers having different chemical composition ratios.
  • the reducing firing time is the same in the reducing firing step, the higher the temperature, the darker and darker the color of the sintered body may be.
  • the contrast of the sintered body color may become darker.
  • the forming step Prior to the forming step, it is made of at least one powder selected from zirconia powder, iron oxide or cobalt oxide, and further comprising a lamination step of laminating in the mold so that the composition ratio of each powder is formed in at least two layers different from each other; Can be.
  • oxygen may be further supplied to the reducing firing gas.
  • Dental zirconia sintered body for achieving the object of the present invention comprising a redox oxide as a coloring agent, when the redox oxide contained in the sintered body in a weight ratio of 100 to 1 to 30 of the reduced metal oxide in the redox oxide It may be included in the weight ratio range.
  • the redox oxide may include at least one of iron oxide and cobalt oxide, and the reduced metal oxide may include at least one of divalent iron oxide and divalent cobalt oxide.
  • the sintered compact may include 1 wt% or less of redox oxide.
  • the color from one end of the sintered body of the zirconia to the other end may have a gradation of gradation.
  • At least one selected from a firing temperature and a reduced firing gas partial pressure may be applied to a part of the sintered body differently from other parts, so that a part of the sintered body may have a different color from the other part.
  • the color of the zirconia sintered body may be grayed out by differently applying at least one selected from a firing temperature and a reduced firing gas partial pressure for each part of the sintered body.
  • the present invention it is possible to express a color similar to natural teeth by changing only the firing conditions of a molded product having a uniform composition, thereby simplifying a process and a manufacturing apparatus, thereby providing a manufacturing method that is effective in reducing manufacturing cost and shortening manufacturing time.
  • the zirconia produced by this manufacturing method contains a redox oxide, and it was confirmed that the color changes as the amount of the reducing metal oxide increases.
  • the zirconia sintered body according to the present invention may exhibit similar gradations to natural teeth, it may exhibit a natural aesthetic effect when applied to natural teeth in the form of implants, crowns and tooth bridges.
  • Example 1 is a graph of Raman analysis results according to reducing firing conditions according to Example 1.
  • Example 2 is a graph of Raman analysis results according to reducing firing conditions according to Example 2.
  • Example 3 is a graph of Raman analysis results according to reducing firing conditions according to Example 3.
  • the present invention relates to the redox oxide as a coloring agent in the production of natural tooth color in zirconia when artificial zirconia blocks are manufactured, and the chromaticity of the redox oxide increases with increasing reduction metal oxide. It is characteristic to use atmosphere.
  • colored zirconia blocks are prepared by mixing oxides such as iron or cobalt which are redox oxides with zirconia powder.
  • the present invention may further include a material capable of changing the light transmittance of the block together with a material expressing color to implement a change in light transmittance close to a natural tooth.
  • the zirconia block according to the present invention can obtain various colors even in the same composition by changing the firing conditions of the reducing firing atmosphere, and due to these characteristics, there is an advantage that a gradation similar to natural teeth can be obtained while simplifying the stacking of raw materials. .
  • the zirconia block of the present invention is composed of 3Y-TZP (3 mol% Y 2 O 3 -Tetragonal Zirconia Polycrystal) and Fe 2 O 3 , CeO 2 , Er 2 O 3 , and Co 2 O 3 as main components. It consists of a subcomponent containing any one or more substances selected from.
  • Fe 2 O 3 is a shade additive to implement yellow
  • CeO 2 is an additive to implement a light yellow shade
  • Er 2 O 3 a shade additive to implement pink
  • Vita shade guides have been generally used as a method of expressing the color of teeth, and zirconia is also manufactured by mixing according to the raw material mixing ratio determined according to the color code of each vita shade.
  • the color code is largely divided into A, B, C, and D series, and each series is additionally divided into 1 ⁇ 4 levels.
  • Koreans are known to have the most tooth color of A2 ⁇ A3.5.
  • Tosoh's Zpex series which is widely used as a powder for dental zirconia, was used.
  • the characteristics of the Zpex powder used in the present invention are as follows.
  • composition of the Zpex powder is as follows.
  • Combinations of the powders for obtaining the color of the vita shade guide in a general small atmosphere using the Zpex grade powders are as follows.
  • the conventional zirconia production was fired in an oxidizing atmosphere, which is a general minor component atmosphere.
  • the zirconia could be manufactured by mixing a predetermined raw material, but in order to express various colors of natural teeth, There was a problem to find a variety of composition ratio accordingly, if there is a difference between the tooth color after firing was prepared by adjusting the composition ratio again, or there is the trouble of additional firing by coloring additional coloring composition.
  • much more processing steps were required to express the steps such as gradation of teeth like natural teeth.
  • the research was conducted on a method of changing the color of the zirconia of the same raw material mixture by controlling the atmosphere of reducing firing.
  • Each vita shade used in the present invention used a composition having a compounding ratio corresponding to A2, A3.5, A4 and B3 color codes as shown in Table 2.
  • the raw material powder according to the blending ratio is filled in a mold and then pressurized to form a molded body.
  • the molded body was first baked at 1540 ° C. for 4 hours in an oxidizing atmosphere.
  • a reducing firing step using secondary firing was carried out in the reducing element component crisis.
  • the calcination furnace used in the reducing firing step was used as a quartz tube furnace, and after the temperature was raised to 800 to 1300 ° C. at a heating rate of 600 ° C./hr, the mixture was cooled to 10 to 240 minutes.
  • Nitrogen gas was used as the reducing gas, and other reducing gas such as argon gas and hydrogen gas may be used.
  • Reducing gas was supplied at 200 ⁇ 300cc / m 3 per minute, it may vary depending on the size and type of the kiln. The reducing atmosphere was adjusted while flowing a small amount of oxygen in addition to the reducing gas.
  • the temperature at the time of secondary firing was 800 to 1300 ° C.
  • it is 1000-1300 degreeC.
  • the secondary firing temperature is lower than 1000 °C, the reduction firing reaction rate is too slow, the overall firing time was long, and when the secondary firing temperature is higher than 1300 °C, the reaction rate is too fast, the color change by the reduction reaction is rapidly progressed Was difficult to control with color.
  • the color change is changed to a darker color than that of the zirconia sintered body after the primary firing. In other words, as the firing temperature increases in the reducing firing atmosphere, the contrast of the color becomes dark, and when the other conditions such as temperature are the same, the darkness becomes darker as time increases.
  • the specimen of A2 composition can be changed to a variety of colors between A2 and A3.5 depending on the reducing conditions when subjected to secondary firing, which is a reducing firing atmosphere. This change in color was also confirmed in other specimens such as A3.5 and A4, and it is expected that the control of the firing conditions may be possible in the reducing firing of most zirconia moldings containing iron and cobalt.
  • the most easily controllable factors were temperature, reaction time and reducing gas partial pressure.
  • the remaining factors were fixed and color adjustment was easy when only one was changed. That is, the temperature and reducing gas partial pressure are fixed, and only the reaction time is changed, or the reaction time and reducing gas partial pressure are fixed, and only the temperature is changed.
  • the intermediate layer is a powder mixed with A2 and A3.5 in a 1: 1 ratio.
  • the photo after reduction firing are compared. Direct illumination is difficult because the lighting environment on the figure is different, but in fact, after reduction firing, the A2 layer is changed similar to the color of A3.5, and the A3.5 layer is similar to the color of B4. In addition, even though only three layers were used, gray scales were naturally formed.
  • the color change of the zirconia in the reducing firing atmosphere is caused by the change of trivalent ions of iron or cobalt into the divalent iron or cobalt in the small amount of iron and cobalt ionic hydride in the zirconia reducing firing atmosphere. It is a phenomenon. This change is made first from the surface of the zirconia fired body and gradually diffuses into the sintered body over time.
  • Redox oxide in the zirconia sintered body is preferably included 1% by weight or less.
  • redox oxide is included in more than 1% by weight, the color not only shows a lot of difference from the color of natural teeth, but also becomes difficult to apply as an artificial tooth since it is changed to a color close to black after reducing firing.
  • the zirconia molded body having a uniform composition ratio it is also possible to partially change the color of the zirconia molded body having a uniform composition ratio by changing the color as the conditions of the reducing firing are changed.
  • one side portion may be fired at 800 ° C., and the opposite side portion may be fired at 1300 ° C., thereby enabling the multishade to be implemented without using a molded body having a different composition ratio.
  • Tosoh Zpex powder was used, and as shown in Table 3, Zpex 57.85%, Zpex-Yellow 40.00%, and Zpex-Pink 2.15% were mixed and filled into a mold by pressing to form a molded body.
  • the molded body was first baked at 1540 ° C. for 4 hours in an oxidizing atmosphere.
  • secondary firing was carried out in the reducing element component crisis.
  • the firing furnace used for the second firing was a quartz tube furnace, and the temperature was raised to 1000, 1100, and 1200 ° C. at a heating rate of 600 ° C./hr, respectively, and maintained at 10, 50, and 70 minutes at the respective temperatures. Then cooled.
  • Reducing gas was supplied at 300 cc / m 3 per minute.
  • the reducing atmosphere was adjusted while flowing a small amount of oxygen in addition to the reducing gas.
  • Raman analysis was performed with specimens with only primary firing.
  • the Raman analysis of the A2 sintered body is shown in FIG. 2.
  • Raman analysis results showed that most of the major peaks observed in similar positions, 437.8 cm -1 and 1000.4 cm - was formed in the first main peak.
  • the main peak of 438 cm -1 showed stronger strength as the reduction firing time increased.
  • the 438 cm ⁇ 1 peak is a peak related to FeO x , and the degree of reduction of the sintered body through reducing firing can be confirmed.
  • the ratio of Fe 2+ in the total iron oxides according to the time maintained at 1200 ° C. when the A2 sintered body was calcined at 1200 ° C. and reducing elemental atmosphere is as follows.
  • the color was A2.
  • the color of the sintered body which was reduced-fired at 1200 ° C for 10 minutes was similar to A3.5, and the color of the reduced-fired sintered body was similar to B3 for 70 minutes.
  • the color of the reduced-fired sintered body was similar to A4, and it was confirmed that the color was changed to a darker color as the holding time was increased in the same reducing atmosphere.
  • the A2 sintered body was subjected to the same test with a reduced firing temperature of 70 minutes, and the reduced firing temperature was changed to 1000, 1100, and 1200 ° C, respectively. It appeared similar to A3.5, 1100 °C specimens were similar to B3, 1200 °C specimens were similar to A4 showed that the reduction reaction proceeds rapidly and changes to a darker color depending on the temperature.
  • Tosoh's Zpex powder was used. As shown in Table 3, Zpex 53.18%, Zpex-Yellow 43.33%, Zpex-Gray 1.33% and Zpex-Pink 2.15% were mixed in a weight ratio, and then pressurized. A molded article was made. The molded body was first calcined at 1540 ° C. for 4 hours in an oxidizing atmosphere. In order to change the color of the firstly fired fired body, secondary firing was carried out in the reducing element component crisis. The firing furnace used for secondary firing was used as a quartz tube furnace, and the temperature was raised to 1200 ° C. at a heating rate of 600 ° C./hr, and then cooled at 10 and 60 minutes at the maximum temperature. Reducing gas was supplied at 300 cc / m 3 per minute. The reducing atmosphere was adjusted while flowing a small amount of oxygen in addition to the reducing gas. For comparison, Raman analysis was performed with specimens with only primary firing.
  • the Raman analysis of the B3 sintered body is shown in FIG. 3.
  • Raman analysis results showed that most of the major peaks observed in similar positions, 438.1 cm -1 and 1003.1 cm - was formed in the first main peak.
  • the main peak of 438 cm -1 showed stronger strength as the reduction firing time increased.
  • the 438 cm ⁇ 1 peak is a peak related to FeO x , and the degree of reduction of the sintered body through reducing firing can be confirmed.
  • the peak related to CoO was 642.0 cm - 1, and it was confirmed that the intensity increased after reducing firing.
  • the ratio of Fe 2+ and Co 2+ in the total iron oxide and cobalt oxide according to the time maintained at 1200 ° C. when the B3 sintered body was calcined at 1200 ° C. and reducing elemental atmosphere is as follows.
  • Tosoh Zpex powder was used, and as shown in Table 3, Zpex 7.96%, Zpex-Yellow 80.00%, Zpex-Gray 6.67%, and Zpex-Pink 5.38% were mixed in the weight ratio and filled and pressurized.
  • a molded article was made. The molded body was first calcined at 1540 ° C. for 4 hours in an oxidizing atmosphere. In order to change the color of the firstly fired fired body, secondary firing was carried out in the reducing element component crisis. The firing furnace used for secondary firing was used as a quartz tube furnace, and the temperature was raised to 1200 ° C. at a heating rate of 600 ° C./hr, and then cooled at 10 and 60 minutes at the maximum temperature. Reducing gas was supplied at 300 cc / m 3 per minute. The reducing atmosphere was adjusted while flowing a small amount of oxygen in addition to the reducing gas. For comparison, Raman analysis was performed with specimens with only primary firing.
  • the Raman analysis of the A4 sintered body is shown in FIG. 4.
  • Raman analysis results showed that most of the major peaks observed in similar positions, 437.6 cm -1 and 1000.8 cm - was formed in the first main peak.
  • the main peak of 437.6 cm -1 showed a stronger strength as the reduction firing time increased.
  • 437.6 cm -1 peak is a peak related to FeO x can confirm the degree of reduction of the sintered body through reducing firing.
  • the peak related to CoO was 704.5 cm - 1, and it was confirmed that the intensity increased after reducing firing.
  • the ratio of Fe 2+ and Co 2+ in the total iron oxide and cobalt oxide according to the time maintained at 1200 ° C. when the B3 sintered body was calcined at 1200 ° C. and reducing elemental atmosphere is as follows.
  • the zirconia sintered body was always obtained only zirconia sintered body of the same color when the composition ratio is the same in the conventional general oxidizing atmosphere, zirconia of various colors according to the firing conditions when using the reducing firing method of the present invention It is a more advantageous technique to make the color of artificial teeth more similar to natural teeth.

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  • Ceramic Engineering (AREA)
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Abstract

La présente invention est caractérisée par un corps fritté en zircone et un procédé de production d'un corps fritté, le procédé comprenant : une étape de moulage pour former un corps moulé en zircone qui comporte de la zircone en tant que composant principal et comprend un oxyde redox; et une étape de cuisson réductrice de zircone dans laquelle la couleur du corps moulé en zircone est modifiée au moyen de l'inclusion d'un oxyde métallique de réduction dans celui-ci par ajustement d'au moins un élément choisi parmi la température de cuisson, le temps de cuisson, et la pression partielle de gaz de cuisson réductrice dans une atmosphère de cuisson réductrice pour distribuer un gaz de cuisson réductrice dans un four de cuisson.
PCT/KR2016/009484 2016-08-26 2016-08-26 Corps fritté en zircone utilisant une cuisson réductrice et son procédé de production WO2018038295A1 (fr)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001097786A (ja) * 1999-07-29 2001-04-10 Kyocera Corp セラミック部材のマーキング方法とマーキングされたセラミック部材
KR20110076357A (ko) * 2009-12-29 2011-07-06 서울시립대학교 산학협력단 지르코니아의 변색 방법
KR101324467B1 (ko) * 2012-06-12 2013-11-06 (주)에큐세라 다양한 색상과 투광성이 있는 기능성 지르코니아 블록
KR20140056168A (ko) * 2011-07-29 2014-05-09 토소가부시키가이샤 착색 투광성 지르코니아 소결체 및 그의 용도
KR101601948B1 (ko) * 2014-09-16 2016-03-10 주식회사 하스 강도, 투광성,색상 구배를 지닌 치과용 지르코니아 블록 및 이의 제조방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001097786A (ja) * 1999-07-29 2001-04-10 Kyocera Corp セラミック部材のマーキング方法とマーキングされたセラミック部材
KR20110076357A (ko) * 2009-12-29 2011-07-06 서울시립대학교 산학협력단 지르코니아의 변색 방법
KR20140056168A (ko) * 2011-07-29 2014-05-09 토소가부시키가이샤 착색 투광성 지르코니아 소결체 및 그의 용도
KR101324467B1 (ko) * 2012-06-12 2013-11-06 (주)에큐세라 다양한 색상과 투광성이 있는 기능성 지르코니아 블록
KR101601948B1 (ko) * 2014-09-16 2016-03-10 주식회사 하스 강도, 투광성,색상 구배를 지닌 치과용 지르코니아 블록 및 이의 제조방법

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