KR20210113583A - Zirconia powder having black color, laminate pattern ceramic sintered body using the powder, and method for manufacturing the same - Google Patents

Abstract

The present invention relates to a zirconia powder having black color enabling manufacture of sintered ceramic bodies with various colors, a sintered laminate pattern ceramic body using the same, and a manufacturing method thereof. More specifically, the zirconia powder is manufactured by mixing, drying, primary sintering, pulverization, molding, and secondary sintering of a powder in which 92.6 wt% of yttria-stabilized zirconia having a white color, 1.6 wt% of silicon dioxide, 2.8 wt% of aluminum oxide, and 3 wt% of a binder, or 72.6 wt% of zirconia having a white color, 1.6% by weight of silicon, 2.8% by weight of aluminum oxide, 3% by weight of a binder, and 20% by weight of black pigment.

Description

Zirconia powder having black color, laminate pattern ceramic sintered body using the powder, and a method for manufacturing the same

The present invention relates to a zirconia powder having a black color, a laminate pattern ceramic sintered body using the powder, and a method for manufacturing the same, and more particularly, to a zirconia, a starting raw material, by selectively mixing an additional material to selectively give a white color or a black color However, it relates to a technology that suppresses cracking, can exhibit a dense structure, has high strength, and has an excellent effect on the coefficient of thermal expansion.

In general, zirconia ceramics are used as structural materials for artificial joints and teeth, luxury brand watches and jewelry, and as high-end materials for fashion, and are a material that shows excellent toughness, abrasion resistance and high strength. As of 2015, it is estimated to be approximately USD 413.7 billion (domestic market size is approximately KRW 76.9 trillion), and is expected to reach USD 778.5 billion (KRW 241.7 trillion in Korea) by 2025, with an average annual growth rate of 6%.

In order to use zirconia ceramics as a variety of materials, research on the color of zirconia ceramics, which is attracting attention both domestically and internationally, has been conducted, and overseas luxury brands are also producing jewelry using the materials of zirconia ceramics. Accordingly, zirconia ceramics are attracting attention as a high-end fashion material.

Recently, Max Evan Enco, a French zirconia ceramic jewelry brand, recorded sales of 15.4 billion won in 2015, indicating that the possibility of zirconia ceramic jewelry is very high. In addition, sales of Serat and MID, the representative ceramic jewelry and watch manufacturers in Korea, recorded 5 billion and 2 billion won in 2015.

The marketability of the non-gift fashion jewelry market is estimated at KRW 4.175.8 trillion, and the sales of traditional ceramic machinery and other industrial parts, which can be evaluated as ceramic jewelry, are increasing every year.

On the other hand, zirconia ceramics, which have excellent properties of high toughness, high wear resistance, and high strength, have been mainly used as structural materials for industrial use. Pure zirconia has a monoclinic structure that is stable below 1170°C, and a tetragonal structure is stable above 1170–2370°C. The cubic structure is known to be stable above 2370°C.

The greatest characteristic of pure zirconia is that it has a stable monoclinic structure at room temperature, and the density is 5.56 g/m3. Because the volume change of 4.6% is accompanied, cracks occur during cooling even when pure zirconia is sintered and the sintered body is broken.

), 세리아(

), 마그네시아(

)를 첨가하여 결정격자 내의 산소결함을 발생시켜 입방정(cubic)구조로서 안정한 구조로 변화시키는데 이를 안정화 지르코니아 라고 한다.Stabilized zirconia was studied to compensate for the problems of pure zirconia, and yttria (

), Seria (

), magnesia (

) is added to generate oxygen defects in the crystal lattice and change into a stable cubic structure, which is called stabilized zirconia.

Stabilized zirconia is stable up to high temperature, but has low strength and low sinterability, so it cannot be used as a high-strength material. The heads of cubic) and tetragonal structures were mixed. Therefore, even if stress occurs in countless crystals inside the ceramic, the structure of the crystal is changed to withstand the force and external force.

It is reported that this partially stabilized zirconia has a smaller thermal expansion coefficient than that of pure zirconia or stabilized zirconia.

Although a number of techniques for manufacturing sintered compacts using other zirconia as raw materials such as conventional partially stabilized zirconia have been disclosed, cracks are severely generated, a dense structure cannot be represented, and the strength is low and easily broken, while the coefficient of thermal expansion is low. It has a problem that it cannot have an excellent effect.

Korean Patent No. 10-0174653 Korean Patent Publication No. 10-1925215 Korean Patent Publication No. 10-0626721 Korean Patent Publication No. 10-2025712 Korean Patent Publication No. 10-1832527

), 산화알루미늄(

), 바인더 3중량%으로 구성된 화이트색상의 세라믹 소결체 또는 화이트 색상을 갖는 지르코니아를 사용하고, 상기 지르코니아에, 이산화규소(

), 산화알루미늄(

), 바인더 3중량%에 선택적으로 흑색 색상을 갖는 안료를 넣어 블랙 색상을 갖는 세라믹 소결체를 제조할 수 있도록 하여, 크랙발생을 억제하고, 치밀한 조직을 나타낼 수가 있으며, 강도가 높고 열팽창계수에 탁월한 효과를 가지도록 하는 화이트색상 또는 블랙색상을 갖는 지르코니아 파우더와 그 파우더를 이용한 라미네이트 패턴 세라믹 소결체 및 그 제조방법을 두고 그 기술적 과제로 완성해낸 것이다.Therefore, an object of the present invention is to selectively have white or black color so that it can be applied to jewelry, but as a starting material, yttria having a white color with a density of 5.9 g/m3 and a strength of 300 Mpa based on a 3-point strength meter Using stabilized zirconia, to the zirconia, silicon dioxide (

), aluminum oxide (

), using a white ceramic sintered body or zirconia having a white color composed of 3% by weight of the binder, and to the zirconia, silicon dioxide (

), aluminum oxide (

), a black color pigment is selectively added to 3% by weight of the binder so that a ceramic sintered body having a black color can be manufactured, thereby suppressing the occurrence of cracks and exhibiting a dense structure, high strength and excellent effect on the coefficient of thermal expansion It was completed as a technical task with a zirconia powder having a white or black color to have

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%, 흑색 색상을 갖는 안료 20중량%로 구성되는 것을 기술적 특징으로 한다.As a technical idea for achieving the above object, 72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of the binder, and 20% by weight of a pigment having a black color is technically characterized.

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%, 흑색 색상을 갖는 안료 20중량%를 혼합하여 혼합물을 형성한 후, DI Water, 지르코니아볼, 상기 혼합물을 7:2:1로 혼합하여 6시간 동안 혼합하는 파우더혼합단계(S100); 상기 혼합단계에서 혼합된 파우더를 80℃, 8시간 건조하는 건조단계(S200); 상기 건조된 파우더를 분단위로 승온속도 5℃로 1000℃까지 승온하고, 1000℃이후 분단위로 승온속도 2℃로 1250℃까지 승온한 후 자연 냉각하는 제1차소결단계(S300); 상기 1차 소결된 파우더를 분쇄하는 분쇄단계(S400); 상기 분쇄된 파우더를 구비된 몰드에 넣은 후 일축가압 성형기에 100mpa로 가압하여 성형하는 성형단계(S500); 상기 성형된 성형체를 분단위로 승온속도 2℃로 500℃까지 승온한 후 2시간 유지하여 바인더를 모두 날리고, 분단위로 승온속도 5℃로 하여 900℃까지 승온시킨 후 1시간 유지하여 불순물을 제거하며, 분단위 승온속도 5℃로 하여 1100℃에서 1시간 유지하며 성형체의 1차 변형이 일어나도록 하고, 분단위 승온속도 5℃로 하여 1300℃까지 승온하되 1시간 유지하여 성형체의 2차변형이 일어나도록 하며, 분단위 승온속도 2℃로 하여 1400~1450℃까지 승온시킨 후 2~4시간 유지한 다음 자연냉각하는 제2차 소결단계(S600); 로 이루어지는 것을 기술적 특징으로 한다.72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of binder, and 20% by weight of pigment having a black color to form a mixture, DI Water, zirconia balls, and the mixture are mixed in a ratio of 7:2:1 and powder mixed for 6 hours mixing step (S100); A drying step of drying the powder mixed in the mixing step at 80° C. for 8 hours (S200); A first sintering step (S300) of heating the dried powder to 1000°C at a temperature increase rate of 5°C in minutes, and then naturally cooling after raising the temperature to 1250°C at a temperature increase rate of 2°C in minutes after 1000°C; a grinding step of grinding the primary sintered powder (S400); A molding step (S500) of putting the pulverized powder into a provided mold and then pressing it at 100 mpa in a uniaxial pressure molding machine; After raising the temperature of the molded article to 500 °C at a temperature increase rate of 2 °C in minutes, hold it for 2 hours to blow off all the binder, and after raising the temperature to 900 °C at a temperature increase rate of 5 °C in minutes, hold for 1 hour to remove impurities, Set the temperature increase rate in minutes to 5°C and maintain it at 1100°C for 1 hour to cause the primary deformation of the molded body. a second sintering step (S600) of raising the temperature to 1400 to 1450 °C at a temperature increase rate of 2 °C in minutes and maintaining it for 2 to 4 hours and then naturally cooling; It is characterized in that it consists of a technical feature.

According to the zirconia powder having a black color according to the present invention, a laminate pattern ceramic sintered body using the powder, and a method for manufacturing the same, it can be selectively manufactured in a white color or a black color depending on the use to be applied to jewelry, so that the versatility of use is increased. By mixing silicon dioxide and aluminum oxide with zirconia having a white color as a starting material, it is possible to suppress cracking, to exhibit a dense structure, and to have high strength and excellent effect on the coefficient of thermal expansion. It is a useful invention.

1 is a view showing the physical properties of TZ-8Y zirconia powder, which is a starting material of the present invention;
2 is a view showing a white zirconia powder of the present invention;
3 is a view showing a black zirconia powder of the present invention;
Figure 4 is a flow chart for producing the white or black zirconia powder of the present invention
5 is a view showing the raw material mixture of the white zirconia powder of the present invention;
Figure 6 is a view showing the pigment mixing ratio of the black zirconia powder of the present invention Figure 7 is a view showing a comparison of the white color and black ceramic sintered body of the present invention
8 is a view showing the density of the white ceramic sintered body of the present invention;
9 is a view showing the density of the black ceramic sintered body of the present invention;
10 is a view showing the density of the white and black ceramic sintered body of the present invention;
11 is a view showing the strength of the white ceramic sintered body of the present invention;
12 is a view showing the strength of the black ceramic sintered body of the present invention;
13 is a view showing the strength of the white and black ceramic sintered body of the present invention;
14 is a view showing the thermal expansion of the white ceramic sintered body of the present invention;
15 is a view showing the thermal expansion of the black ceramic sintered body of the present invention;
16 is a view showing the thermal expansion of the white and black ceramic sintered body of the present invention;
17 is a view showing the microstructure of the white ceramic sintered body of the present invention;
18 is a view showing the microstructure of the black ceramic sintered body of the present invention;
19 is a view showing a ceramic sintered body in which white or black color and white and black color are combined according to the present invention;
20 is a view showing the sintered body after the polishing operation of the ceramic sintered body of the present invention
21 is a view showing the microstructure of the boundary portion of the sintered body of white and black color;
22 is a view showing the density, strength, and coefficient of thermal expansion of the white or black sintered body of the present invention;

The present invention selectively has white or black color by selectively mixing additional materials with zirconia TZ-8Y, which is a starting material, suppressing crack generation, can exhibit a dense structure, high strength, and excellent effect on coefficient of thermal expansion To provide a zirconia powder having a black color to have a zirconia powder, a laminate pattern ceramic sintered body using the powder, and a method for manufacturing the same.

Hereinafter, with reference to FIGS. 1 to 22, preferred configurations and actions of the present invention for achieving the above object will be described with reference to the accompanying drawings.

On the other hand, by using the yttria-stabilized zirconia having a white color, powder having a white color or a black color, and each powder thereof, a ceramic sintered body having a white color can be obtained.

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%로 구성된다.As shown in the figure, the powder having the white color has a white color as shown in Fig. 92.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight and 3% by weight of the binder.

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%, 블랙 색상을 갖는 안료 20중량%로 구성된다.In addition, the powder having the black color is 72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of binder, and 20% by weight of pigment having a black color.

At this time, in the case of the pigment having the black color, it is a NF-710 pigment used commercially as a pigment capable of expressing a black color at 1400° C. or higher.

)40%, 산화이제철(

)30%, 삼산화삼코발트(

)10%, 마그네시아(

)10%, 산화니켈(NiO)10%의 비율로 구성되어 있다.The ratio of the pigment is chromium oxide (

) 40%, ferric oxide (

) 30%, tricobalt trioxide (

)10%, Magnesia (

) 10% and nickel oxide (NiO) 10%.

In addition, in the steps to be described below, when the laminate pattern ceramic sintered body having the black color was manufactured, the mixing ratio of the pigment was 5 to 20% by weight.

At this time, the mixing ratio of the zirconia having the white color is changed according to the mixing ratio of the pigment.

That is, when the powder having the white or black color is mixed with zirconia (TZ-8Y) used as a starting material, the color of the powder can be determined according to the mixing ratio.

Meanwhile, a method of manufacturing a laminate pattern ceramic sintered body having a white color is as follows with reference to FIG. 4 .

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%를 혼합하여 혼합물을 형성한 후, DI Water, 지르코니아볼, 상기 혼합물을 7:2:1로 혼합하여 6시간 동안 혼합하는 파우더혼합단계를 수행한다.First, 92.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight and 3% by weight of a binder to form a mixture, then DI Water, zirconia balls, and the mixture are mixed at a ratio of 7:2:1 to perform a powder mixing step of mixing for 6 hours.

A drying step of drying the powder mixed in the mixing step at 80° C. for 8 hours is performed.

After performing the first sintering step of heating the dried powder to 1000° at a temperature increase rate of 5°C in minutes, and then naturally cooling the temperature to 1250°C at a temperature increase rate of 2°C in minutes after 1000°C, the first A grinding step of pulverizing the sintered powder is performed.

After that, after putting the pulverized powder into a mold provided, a molding step of molding by pressing at 100 mpa in a uniaxial pressure molding machine is performed, and the temperature of the molded product is raised to 500° C. at a temperature increase rate of 2° C. in minutes for 2 hours. The binder is blown off by holding, and the temperature is raised to 900°C at a rate of 5°C in minutes, and then maintained for 1 hour to remove impurities. The temperature is raised to 1300°C at a temperature increase rate of 5°C in minutes, and maintained for 1 hour to cause secondary deformation of the molded body. By performing the second sintering step of maintaining for 4 hours and then naturally cooling, it is possible to finally obtain a laminate pattern ceramic sintered body using zirconia powder having a white color.

Here, the manufacturing method of the laminate pattern ceramic sintered body having a black color is the same as the manufacturing method of the laminate pattern ceramic sintered body having a white color, but in the initial powder mixing step, the mixing ratio and mixing materials are mixed slightly differently.

) 1.6중량%, 산화알루미늄(

) 2.8중량%, 바인더 3중량%, 흑색 색상을 갖는 안료 20중량%를 혼합하여 혼합물을 형성한 후, DI Water, 지르코니아볼, 상기 혼합물을 7:2:1로 혼합하여 6시간 동안 혼합하는 파우더혼합단계를 수행한다.The method for manufacturing a laminate pattern ceramic sintered body having a black color is 72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of binder, and 20% by weight of pigment having a black color to form a mixture, DI Water, zirconia balls, and the mixture are mixed in a ratio of 7:2:1 and powder mixed for 6 hours A mixing step is performed.

As described above, for the laminate pattern ceramic sintered body using zirconia powder having a white or black color, the experimental results for density, strength, coefficient of thermal expansion, and microstructure are as follows.

, TZ-8Y+

, TZ-8Y+

+

로 4가지로 하여 실험하였다.As an experimental condition, as shown in FIG. 5, a laminate pattern ceramic sintered body having a white color TZ-8Y, TZ-8Y+

, TZ-8Y+

, TZ-8Y+

+

It was tested in 4 ways.

+

+안료를 5~20중량%로 혼합하여 5, 10, 15, 20중량%로 각각 성형된 소결체 4가지로 실험하였다.In addition, as shown in FIG. 6, the laminate pattern ceramic sintered body having a black color is TZ-8Y+

+

The experiment was conducted with 4 sintered bodies formed by mixing the + pigment at 5 to 20% by weight, respectively, at 5, 10, 15, and 20% by weight.

Meanwhile, as shown in FIG. 7 , four types of laminate pattern ceramic sintered bodies having a white color and 4 types of laminate pattern ceramic sintered bodies having a black color were tested with a total of 8 types.

1. Analysis method of the 8 types of ceramic sintered bodies

1) Density measurement method

The density was analyzed using a piconometer density meter, but the density was obtained as P=V/M, and the piconometer is an analytical tool to obtain the density, adopting Archimedes' fluid displacement principle and Boyle's gas expansion law to obtain solid materials. A density meter, a device that can accurately measure the true density of

2) How to measure bending strength

Bending strength measurement is to measure the deformation resistance or breaking strength when a bending moment is applied to the material. tests, etc.

In general, a universal tester is equipped with a device for bending test, and the test piece is supported at points A and B, and the load is applied at the center or at 2 points equidistant from A and B. The former is bent at 3 points, and the latter is at 4 points. It is called bending, and in the three-point bending method, the maximum bending moment moment (Mbmax=Pm/2) is reached at the load point.

Therefore, in three-point bending, cracks occur from the back surface just below the load point, and in the latter case, fracture starts from the weakest defect among the tensile-side surfaces between C and D.

3) Thermal expansion coefficient analysis method

Thermomechanical Analyzer (TMA) Thermomechanical analyzer is a device that measures the size changes due to expansion and contraction as a function of temperature and time by applying a temperature program to the sintered body. is used to measure

The measuring principle is that the dilatometry measurement method has very small load and mechanical stress on the sintered body, but the TMA measurement method measures the expansion and contraction of the sintered compact by applying a Newton load from a load close to zero. The measurement signal uses a linear variable differential transformer (LVDT), and has the advantage of providing very good resolution for the expansion process before and after the glass transition, for example.

In addition, since TMA measures length change as a function of temperature and load, it is very useful for comparative studies of transition phenomena as it is superior to DSC which measures specific thermal change or enthalpy change. In the present invention, the measurement of relative length change was analyzed.

4) Microstructure analysis method

Scanning electron microscope, called SEM, is a kind of electron microscope that scans the surface through an electron beam and images it. When high-speed electrons are fired, these electrons collide with the surface of the sintered body and interact, causing electron-like substances to pop out of the sample. This is an analysis method.

The microstructure of zirconia must be evaluated as an important factor determining the mechanical properties (strength, toughness, low-temperature deterioration, fatigue properties) of the material. Through microstructure observation, the degree of densification and homogeneity of the zirconia material can be evaluated, and the average particle diameter of the material can be obtained.

2. Analysis results of 8 types of ceramic sintered bodies

The following analysis results are consistent with the drawings,

=ZY8S, TZ8Y+

=ZY8A, TZ8Y+

+

=ZY8SA로 하여 설명하기로 하고,4 types of white zirconia TZ8Y=ZY8, TZ8Y+

=ZY8S, TZ8Y+

=ZY8A, TZ8Y+

+

=ZY8SA will be used to explain,

+

+5%=ZY8SA5B, TZ8Y+

+

+10%=ZY8SA10B, TZ8Y+

+

+15%=ZY8SA15B, TZ8Y+

+

+20%=ZY8SA20B로 하여 설명하기로 한다.Four types of black zirconia are TZ8Y+

+

+5%=ZY8SA5B, TZ8Y+

+

+10%=ZY8SA10B, TZ8Y+

+

+15%=ZY8SA15B, TZ8Y+

+

+20% = ZY8SA20B will be described.

1)Piconometer milled measurement result

Density is related to sinterability as shown in FIG. 10, and the densities of ZY8, ZY8S, ZY8A, ZY8SA of the white ceramic sintered body and ZY8SA5B, ZY8SA10B, ZY8SA15B, and ZY8SA20B of the black colored ceramic sintered body were measured.

As shown in FIG. 8, the theoretical density of ZY8 of white color is 5.9 g/m3, and as a result of the experiment, the density of ZY8SA was most similarly measured as the theoretical density of 5.9 g/m3.

As shown in FIG. 9 , the black color was measured the highest in ZY8SA5B at 5.57 g/m3 and ZY8SA15B at 5.57 g/m3.

The overall sinterability of the white color ranged from 96% to 104%, and the overall sinterability of the black color ranged from 92% to 95%, and it can be seen that most of the sintering was well done.

2) Bending strength measurement result

As shown in FIG. 13, the strength measurements of ZY8, ZY8S, ZY8A, ZY8SA raw materials of white color and ZY8SA5B, ZY8SA10B, ZY8SA15B, and ZY8SA20B of black color were shown, as shown in FIG. 13 .

As shown in FIG. 11 , as for the white color, the ZY8SA was measured to be the highest at 98Mpa, and for the black color, as shown in FIG. 12 , the ZY8SA20B was measured to be the highest at 48.5Mpa.

3) TMA coefficient of thermal expansion measurement result

The most important indicator in the present invention is the TMA coefficient of thermal expansion analysis. When the laminate pattern ceramic is sintered, if the coefficients of thermal expansion are different, cracks may occur, making it difficult to produce a stable sintered body. It was measured based on the measurement of the relative length change during the coefficient of thermal expansion analysis.

As shown in FIG. 16, the measurement result of the thermal expansion coefficient of the entire sintered body is shown, and as shown in FIG. 14, the measurement result of the change in the length of the thermal expansion coefficient of white color is shown, and the length change of the finally selected ZY8SA is 1.493 mm. was measured.

As shown in FIG. 15 , the measurement result of the change in the length of the thermal expansion coefficient of black color is shown, and the change in length of the ZY8SA20B was measured to be 1.493 mm.

As a result of the measurement, the length change of the coefficient of thermal expansion of ZY8SA and ZY8SA20B was measured to coincide.

4) SEM microstructure analysis result

The cross-sectional microstructure of ZY8SA, a sintered body of white color selected based on the change in the length of the thermal expansion coefficient, which is an important indicator in the composition design study of the laminate pattern, was shown as shown in FIG. 17, and the cross-sectional microstructure of ZY8SA20B is shown in FIG. It was uniformly distributed as shown, and showed a relatively dense structure.

5) Analysis of laminate pattern ceramic sintered body

As shown in FIG. 22 , the results of measuring the density, strength, and coefficient of thermal expansion of white zirconia and black zirconia showed that the physical properties and thermal expansion coefficient of ZY8SA and that of ZY8SA20B were the best.

When sintering ZY8SA of white color and ZY8SA20B of black color under the sintering conditions of the present invention, a sintered body that does not generate cracks as shown in FIG. 19 was produced, and as shown in FIG. 20, it was made of stone.

In addition, as shown in FIG. 21 , as a result of analyzing the microstructure of the interface between the white color and the black color in the bulk of the laminate pattern ceramics, an even microstructure was shown and a relatively dense structure was shown.

In the present invention, the composition of laminated pattern ceramics of different colors was designed under the condition that cracks do not occur, and the final white color ZY8SA and black color ZY8SA20B were uniaxially pressed and then sintered to show a stable bulk shape.

Based on the manufacturing method and experimental results of the present invention, it became possible to manufacture zirconia ceramic sintered bodies having various colors.

According to the zirconia powder having a white or black color according to the present invention, a laminate pattern ceramic sintered body using the powder and a method for manufacturing the same, it can be selectively manufactured in a white color or black color depending on the intended use to be applied to jewelry. By mixing silicon dioxide and aluminum oxide with zirconia having a white color as the starting material, the variety of It is an invention.

Claims (3)

72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) Zirconia powder having a black color, characterized in that it is composed of 2.8% by weight, 3% by weight of a binder, and 20% by weight of a pigment having a black color. 72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of binder, and 20% by weight of pigment having a black color to form a mixture, DI Water, zirconia balls, and the mixture are mixed in a ratio of 7:2:1 and mixed for 6 hours mixing step;
a drying step of drying the powder mixed in the mixing step at 80° C. for 8 hours;
A first sintering step of heating the dried powder to 1000°C at a temperature increase rate of 5°C in minutes, and then naturally cooling the temperature to 1250°C at a temperature increase rate of 2°C in minutes after 1000°C;
pulverizing step of pulverizing the first sintered powder;
A molding step of putting the pulverized powder into a provided mold and then pressing it at 100 mpa in a uniaxial pressure molding machine;
After raising the temperature of the molded article to 500 °C at a temperature increase rate of 2 °C in minutes, hold it for 2 hours to blow off all the binder, and after raising the temperature to 900 °C at a temperature increase rate of 5 °C in minutes, hold for 1 hour to remove impurities, Set the temperature increase rate in minutes to 5°C and maintain it at 1100°C for 1 hour to cause the primary deformation of the molded body. a second sintering step of raising the temperature to 1400 to 1450 °C at a temperature increase rate of 2 °C in minutes, maintaining the temperature for 2 to 4 hours, and then naturally cooling; A method for manufacturing a laminate pattern ceramic sintered body using zirconia powder having a black color, characterized in that consisting of 72.6 wt% of yttria-stabilized zirconia having a white color, silicon dioxide (

) 1.6 wt%, aluminum oxide (

) 2.8% by weight, 3% by weight of binder, and 20% by weight of pigment having a black color to form a mixture, DI Water, zirconia balls, and the mixture are mixed in a ratio of 7:2:1 and mixed for 6 hours mixing step;
a drying step of drying the powder mixed in the mixing step at 80° C. for 8 hours;
A first sintering step of heating the dried powder to 1000°C at a temperature increase rate of 5°C in minutes, and then naturally cooling the temperature to 1250°C at a temperature increase rate of 2°C in minutes after 1000°C;
pulverizing step of pulverizing the first sintered powder;
A molding step of putting the pulverized powder into a provided mold and then pressing it at 100 mpa in a uniaxial pressure molding machine;
After raising the temperature of the molded article to 500 °C at a temperature increase rate of 2 °C in minutes, hold it for 2 hours to blow off all the binder, and after raising the temperature to 900 °C at a temperature increase rate of 5 °C in minutes, hold for 1 hour to remove impurities, Set the temperature increase rate in minutes to 5°C and maintain it at 1100°C for 1 hour to cause the primary deformation of the molded body. a second sintering step of raising the temperature to 1400 to 1450 °C at a temperature increase rate of 2 °C in minutes, maintaining the temperature for 2 to 4 hours, and then naturally cooling; A laminate pattern ceramic sintered body using zirconia powder having a black color, characterized in that it is manufactured and configured with

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