KR100234003B1 - Stabilized zirconia sintered body - Google Patents

Stabilized zirconia sintered body Download PDF

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KR100234003B1
KR100234003B1 KR1019960073598A KR19960073598A KR100234003B1 KR 100234003 B1 KR100234003 B1 KR 100234003B1 KR 1019960073598 A KR1019960073598 A KR 1019960073598A KR 19960073598 A KR19960073598 A KR 19960073598A KR 100234003 B1 KR100234003 B1 KR 100234003B1
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yttria
alumina sol
zirconia
stabilized zirconia
powder
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KR19980054437A (en
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임경란
김소진
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박호군
한국과학기술연구원
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    • C04B2235/3244—Zirconium oxides, zirconates, hafnium oxides, hafnates, or oxide-forming salts thereof
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Abstract

본 발명은 단사정형 지르코니아에 소량의 이트리아와 알루미나를 분말이 아닌 용액으로 첨가함으로써 부분 안정화 지르코니아 소결체를 제조하는 방법에 관한 것으로, 단사정 지르코니아 슬러리에, 이트리아 및 알루미나졸 혼합용액을 첨가ㆍ혼합하고, 상기 슬러리로부터 용매를 제거한 후, 건조하거나 또는 건조, 하소한 후 성형체를 얻고 열처리하는 부분 안정화 지르코니아 소결체의 제조방법을 제공하고, 여기서 상기 이트리아 및 알루미나졸 혼합용액은, 알루미나졸에 이트리아 분말을 첨가하여 용해시킴으로써 얻어질 수도 있고, 또한 이트리아 분말을 산성용액에 녹인 후, 알루미나 졸을 첨가함으로써 얻어질 수도 있고, 또한, 상기 하소는 유기물과 수분을 제거할 수 있는 온도범위인 400 - 700℃에서 행해지는 것이 바람직하다.The present invention relates to a method for producing a partially stabilized zirconia sintered body by adding a small amount of yttria and alumina to a monoclinic zirconia as a non-powder solution, and adding and mixing a mixture of yttria and alumina sol to a monoclinic zirconia slurry. And removing the solvent from the slurry, and then drying or drying and calcining to obtain a molded body and heat treatment. The method provides a method for producing a partially stabilized zirconia sintered body, wherein the mixture of yttria and alumina sol is yttria in alumina sol. It may be obtained by dissolving the powder by adding it, or may be obtained by dissolving the yttria powder in an acidic solution and then adding an alumina sol. The calcining may also be carried out at a temperature range in which organic matter and water can be removed. It is preferable to carry out at 700 degreeC.

Description

부분 안정화 지르코니아 소결체의 제조방법Manufacturing method of partially stabilized zirconia sintered body

본 발명은 단사정형 지르코니아에 소량의 이트리아와 알루미나를 분말이 아닌 용액으로 첨가함으로써 부분 안정화 지르코니아(PSZ : Partially Stabilized Zirconia)소결체를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a partially stabilized zirconia (PSZ: Partially Stabilized Zirconia) sintered body by adding a small amount of yttria and alumina to a monoclinic zirconia as a solution rather than a powder.

일반적으로 지르코니아는 단사정 (monoclinic), 정방정 (tetragonal) 및 입방정 (cubic) 형태의 세 가지 동소체로 존재하고 있다. 낮은 온도에서 존재하는 단사정 지르코니아는 고온에서 정방정형 또는 입방정형으로 상 변화에 따라 안정한 소결체로 변화하나 저온에서 다시 단사정형 지르코니아로 되돌아오기 때문에 사용할 수 없다. 상기 PSZ는 100 ~ 200℃온도에서 장시간 습기 중에 노출될 때에는 단사정으로 상 전이가 일어나 재료표면에 미세 균열을 발생하는, 소위 저온열화 현상을 나타내기 때문에 단일암체로 사용할 수 없다.In general, zirconia exists in three allotropes in the form of monoclinic, tetragonal, and cubic. Monoclinic zirconia present at low temperature is changed to stable sintered body with phase change from tetragonal or cubic to high temperature, but cannot be used because it returns to monoclinic zirconia at low temperature. The PSZ cannot be used as a single rock body because it exhibits a so-called low temperature deterioration phenomenon, in which phase transition occurs in a monoclinic when exposed to moisture at a temperature of 100 to 200 ° C. for a long time, causing microcracks on the material surface.

일반적으로 상기 현상을 방지하기 위한 방법으로 입방정 또는 정방정 지르코니아의 상을 안정화하기 위한 별도의 안정화제가 요구된다. 이러한 안정화제로는 Y2O3, CaO, MgO, CeO2등의 산화물이 알려져 있다. 그러나 일반적으로 널리 이용되는 고상법에는 이러한 안정화제를 균일하게 분산시키기가 매우 힘들어 사용되고 있지 않다. 이의 개선책으로 지르코니아 분말 제조시 안정화제를 첨가하여 안정화 지르코니아 분말을 제조한다. 안정화 지르코니아라는 용어는 지르코니아에 상기 기술한 안정화제를 첨가하여 고온에서는 물론 저온에서도 지르코니아를 안정화시킨 것으로 정의할 수 있다. 시판되는 안정화 정방정 지르코니아 분말에는 이트리아가 지르코니아에 대해 2 - 4 몰%가 포함되어 있다. 이 안정화 지르코니아 분말은 1400 ~ 1600℃에서 소결하면 부분 안정화 지르코니아 (PSZ) 소결체를 얻을 수 있다. 이 이트리아 안정화 지르코니아는 비교적 기계적 특성이 좋기 때문에 가장 많이 사용되고 있으므로 이와 관련된 많은 기술 문헌을 볼 수 있다. 여컨대 미국 특허 제 4, 886, 768호에서는 3 몰%의 이트리아로 안정화된 지르코니아에 5가 산화물을 첨가제로 사용하는 내용을 개시하고 있으나, 실제 적용시 재료의 신뢰성에 영향을 미치는 저온열화에 문제가 있는 것으로 사료된다. 한편 미국 특허 제 5, 008, 221호에는 상기 인용 특허와 마찬가지로 Y2O3가 2 ~4 몰%, Nb2O5나 Ta2O5가 0.5 ~ 3.0몰% 포함하는 내용을 개시하고 있으나, 이것 역시 저온열화에 대해 아무런 언급을 하고 있지 않아 지르코니아 소결체 사용에 문제가 있는 것으로 유추된다.In general, a separate stabilizer for stabilizing the phase of the cubic or tetragonal zirconia is required as a method for preventing the phenomenon. As such stabilizers, oxides such as Y 2 O 3 , CaO, MgO, CeO 2 and the like are known. However, in the solid phase method that is widely used in general, it is very difficult to uniformly disperse such a stabilizer is not used. As a countermeasure thereof, a stabilizer is added to prepare a zirconia powder to prepare a stabilized zirconia powder. The term stabilized zirconia can be defined as the addition of the stabilizer described above to zirconia to stabilize the zirconia at high temperature as well as low temperature. Commercially available stabilized tetragonal zirconia powder contains 2-4 mol% yttria relative to zirconia. When this stabilized zirconia powder is sintered at 1400 to 1600 ° C., a partially stabilized zirconia (PSZ) sintered body can be obtained. This yttria stabilized zirconia is the most used because of its relatively good mechanical properties, and thus many technical literatures are available. For example, U.S. Patent Nos. 4, 886 and 768 disclose the use of pentavalent oxide as an additive in zirconia stabilized with 3 mol% of yttria. It seems to be a problem. US Patent Nos. 5, 008 and 221 disclose contents containing 2 to 4 mol% of Y 2 O 3 and 0.5 to 3.0 mol% of Nb 2 O 5 or Ta 2 O 5 as in the cited patents. It is also inferred that there is a problem in the use of zirconia sinter since there is no mention of low temperature degradation.

안정화 지르코니아 분말 제조에는 안정화제 외에 ZrOCl2, YCl3등의 무기염 수용액을 수산화 암모니아 등의 염기로 공침전시켜 얻은 침전물을 여과, 세척, 건조 및 열처리 과정을 거쳐 제조하고 있으나, 이트리아가 첨가된 지르코니아 분말이 상기의 물리적 특성 때문에 이트리아가 첨가되지 않은 단사정 지르코니아 분말 보다 가격이 3 - 4 배가 고가로 거래되는 것이 당연하다고 하겠다.In the preparation of stabilized zirconia powder, precipitates obtained by coprecipitation of inorganic salts such as ZrOCl 2 and YCl 3 with a base such as ammonia hydroxide in addition to stabilizers are prepared through filtration, washing, drying, and heat treatment. Due to the physical properties of zirconia powder, it is natural that the price is 3-4 times higher than monoclinic zirconia powder without yttria.

또한, 한국특허공보 제 1993-5318호(공고일자 : 1993. 6. 17.)는 지르코니아에 안정화제 역할의 이트리아를 분말로 첨가하거나, 산에 녹여 첨가하여 균열이 없는 단일암체를 제조하는 방법을 개시하고 있다.In addition, Korean Patent Publication No. 1993-5318 (published date: June 17, 1993) discloses a method for producing a single rock body without cracks by adding yttria as a stabilizer to zirconia as a powder or by dissolving it in an acid. Is starting.

본 발명은 상술한 종래기술이 갖는 문제점을 해결하는 것을 목적으로 한다.The present invention aims to solve the problems of the above-described prior art.

이에, 본 발명은, 단사정 지르코니아 슬러리에, 이트리아 및 알루미나졸 혼합용액을 첨가ㆍ혼합하고, 상기 슬러리로부터 용매을 제거한 후, 건조하거나 또는 건조, 하소한 후 성형체를 얻고 열처리하는 부분 안정화 지르코니아 소결체의 제조방법을 제공한다.Accordingly, the present invention provides a partially stabilized zirconia sintered body in which a mixture of yttria and alumina sol is added and mixed with a monoclinic zirconia slurry to remove a solvent from the slurry, followed by drying or drying and calcining to obtain a molded body and heat treatment. It provides a manufacturing method.

여기서 상기 이트리아 및 알루미나졸 혼합용액은, 알루미나졸에 이트리아 분말을 첨가하여 용해시킴으로써 얻어질 수도 있고, 또한 이트리아 분말을 산성용액에 녹인 후, 알루미나 졸을 첨가함으로써 얻어질 수도 있다.Here, the yttria and alumina sol mixed solution may be obtained by adding and dissolving yttria powder in the alumina sol, or may be obtained by dissolving the yttria powder in an acidic solution and then adding an alumina sol.

또한, 상기 상기 하소는 유기물과 수분을 제거할 수 있는 온도범위인 400 - 700℃에서 행해지는 것이 바람직하다.In addition, the calcination is preferably carried out at 400 to 700 ℃ temperature range that can remove the organic matter and water.

본 발명에 따르면, 이트리아를 알루미나 졸과 반응시켜 일종의 이트리아-알루미나졸을 형성하게 하여 이트리아가 알루미나와 반응하여 950℃에서 Al2O3- Y2O3(Yag)를 형성하기 전에 이트리아가 지르코니아와 반응하여 이트리아-지르코니아 고용체를 만들고 남는 알루미나는 소결 중 지르코니아 입자성장을 억제하여 물성을 증가시키는데 기여하게 된다. 이 때에 사용되는 이트리아량은 지르코니아에 대해 2 ~ 4 몰%이며, 알루미나량도 지르코니아에 대해 1 ~ 5 무게%이다, 알루미나 없이 이트리아 수용액을 이용하여 제조된 소결체는 소결밀도가 이론밀도의 96% 이상으로 높으나, 미세구조의 곳곳에 30 ~ 50μm의 단사정상으로 뭉친 곳이 있으며, 그곳에는 균열이 나타나게 되므로 기대되는 물성의 지르코니아 소결체를 제조할 수 없다.According to the present invention, yttria is reacted with alumina sol to form a kind of yttria-alumina sol so that yttria reacts with alumina before forming Al 2 O 3 -Y 2 O 3 (Yag) at 950 ° C. Tria reacts with zirconia to form yttria-zirconia solid solution, and the remaining alumina contributes to the increase of physical properties by inhibiting zirconia particle growth during sintering. At this time, the amount of yttria used is 2 to 4 mol% with respect to zirconia, and the amount of alumina is also 1 to 5 wt% with respect to zirconia. The sintered compact manufactured using aqueous solution of yttria without alumina has a sintered density of 96 Higher than%, but the microstructures are gathered in a monoclinic phase of 30 ~ 50μm, there is a crack appears there can not produce the expected zirconia sintered physical properties.

본 발명에서 보여주는 알루미나 - 이트리아 복합 졸을 사용하는 방법으로 제조된 지르코니아 분말은 1400 ~ 1600℃의 소결 온도에서 2시간 열처리하면 사용한 단사정 지르코니아 입자크기에 따라 단사정상의 양이 다르다. 즉, 입자가 작으면 100% 단사정상을 보여주며 95% 이상의 상대 소결밀도를 보여준다. 이러한 지르코니아 소결체는 균일한 미세구조를 나타내며 지르코니아 입자크기는 0.5 ~ 1.0μm이 대부분을 이루며 1.5 ~ 2.0μm의 입자들도 약간 섞여 있다. 그러나 알루미나의 입자 크기는 대부분이 0.5 ~ 1.0μm로 이루어진다.The zirconia powder prepared by the method using the alumina-yttria composite sol shown in the present invention is different in monoclinic phase according to the monoclinic zirconia particle size used after heat treatment for 2 hours at a sintering temperature of 1400 ~ 1600 ℃. That is, small particles show a 100% monoclinic phase and a relative sintered density of 95% or more. The zirconia sintered body has a uniform microstructure, and the zirconia particle size is 0.5 to 1.0 μm, and most of the 1.5 to 2.0 μm particles are mixed. However, the particle size of alumina is mostly 0.5 to 1.0 μm.

다음 실시예는 본 발명을 더욱 상세히 예증하여 줄 것이나 본 발명이 여기에 국한 한다는 것은 아니다.The following examples will illustrate the present invention in more detail, but the invention is not limited thereto.

[실시예 1]Example 1

적정량의 알루미나 졸을 약 50℃로 가온하고 여기에 적정량의 이트리아 분말을 조금씩 첨가하고 교반하여 녹인 후 맑은 용액이 되면 30분 더 교반하고 식힌다. 이 알루미나-이트리아 졸을 24시간 볼 밀을 혼합한 m-ZrO2(d50= 0.71μm, d90= 10.26μm)슬러리에 첨가한 후 30분 다시 볼 밀을 혼합하고 건조(100℃, 5시간)하였다.The appropriate amount of alumina sol is warmed to about 50 ° C, and an appropriate amount of yttria powder is added thereto little by little, and then dissolved by stirring. After a clear solution, the solution is stirred for 30 minutes and cooled. The alumina-yttria sol was added to a slurry of m-ZrO 2 (d 50 = 0.71 μm, d 90 = 10.26 μm) mixed with a ball mill for 24 hours, and then the ball mill was mixed again for 30 minutes and dried (100 DEG C, 5). Time).

건조된 분말은 선택적으로 분당 10℃ 승온하여 500℃에서 2시간 하소한 후 100 메쉬체로 거른 후, 1 톤/cm2압력하에 성형체를 만든 다음, 분당 10℃로 승온하여 1500 ~ 1600℃에서 2시간 소결하였다. 표 1 에는 건조만을 행한 경우와 건조 후 하소도 행한 경우를 나누어 보여주고 있다.The dried powder is optionally heated to 10 ° C. per minute, calcined at 500 ° C. for 2 hours, filtered to 100 mesh sieves, made into molded bodies under 1 ton / cm 2 pressure, and then heated to 10 ° C. per minute to 2 hours at 1500 to 1600 ° C. Sintered. Table 1 divides the case where only drying is performed and the case where calcining after drying is also performed.

소결밀도는 알키메데스 원리를 이용하여 증류수에서 잠금법에 의해 측정하였다. 이트리아와 알루미나양에 따른 소결밀도를 표 1에 나타낸다.The sintered density was measured by the locking method in distilled water using the Alchemedes principle. Table 1 shows the sintered density according to the amount of yttria and alumina.

[실시예 2]Example 2

포름 산으로 증류수의 pH를 1.7 ~ 1.9이 되게 조정한 후 이 산성용액을 약 50℃로 가온하고 여기에 3.18몰%에 해당하는 이트리아를 녹인 후, 맑은 용액이 되면 실온으로 식힌다. 여기에 1 ~ 4.1 무게%의 알루미나량에 해당하는 알루미나 졸을 첨가하고 교반하였다. 이 혼합 졸을 24시간 볼 밀로 혼합한 단사정형 지르코니아 슬러리에 첨가한 후 실시예 1과 같은 방법으로 처리하여 소결체를 얻었다. 알루미나량이 소결에 미치는 영향을 표 2에 나타낸다.The pH of the distilled water is adjusted to 1.7 to 1.9 with formic acid. The acidic solution is then warmed to about 50 ° C., dissolved in 3.18 mol% of yttria, and cooled to room temperature. An alumina sol corresponding to the amount of alumina of 1 to 4.1% by weight was added thereto and stirred. This mixed sol was added to a monoclinic zirconia slurry mixed with a ball mill for 24 hours, and then treated in the same manner as in Example 1 to obtain a sintered body. Table 2 shows the effect of the amount of alumina on the sintering.

[비교예 1]Comparative Example 1

이트리아를 포름 산으로 산성화시킨 증류수(pH 1.8)에 녹인 맑은 용액을 24시간 볼 밀로 혼합한 m-ZrO2에 첨가하여 30분 더 볼 밀로 혼합한 후 이 슬러리를 실시예 1과 같은 방법으로 처리하여 소결체를 제조하였다. 이들 소결밀도는 표 3과 같다.A clear solution of yttria acidified with distilled water (pH 1.8) acidified with formic acid was added to m-ZrO 2 mixed with a ball mill for 24 hours, mixed with a ball mill for another 30 minutes, and the slurry was treated in the same manner as in Example 1. To obtain a sintered body. These sintered densities are shown in Table 3.

Claims (4)

단사정 지르코니아 슬러리에, 이트리아 및 알루미나졸 홉합용액을 첨가ㆍ혼합하고, 상기 슬러리로부터 용매를 제거한 후, 건조하거나 또는 건조, 하소한 후 성형체를 얻고 열처리하는 것을 특징으로 하는 부분 안정화 지르코니아 소결체의 제조방법.Preparation of partially stabilized zirconia sintered body comprising adding and mixing a yttria and alumina sol mixed solution to the monoclinic zirconia slurry, removing the solvent from the slurry, and drying or drying and calcining to obtain a molded body and heat treatment. Way. 제1항에 있어서, 상기 이트리아 및 알루미나졸 혼합용액은, 알루미나졸에 이트리아 분말을 첨가하여 용해시킴으로써 얻어지는 것을 특징으로 하는 부분 안정화 지르코니아 소결체의 제조방법.The method for producing a partially stabilized zirconia sintered compact according to claim 1, wherein the mixture of yttria and alumina sol is obtained by adding and dissolving yttria powder to the alumina sol. 제1항에 있어서, 상기 이트리아 및 알루미나졸 혼합용액은, 이트리아 분말을 산성용액을 녹인 후, 알루미나 졸을 첨가함으로써, 얻어지는 것을 특징으로 하는 부분 안정화 지르코니아 소결체의 제조방법.The method for producing a partially stabilized zirconia sintered body according to claim 1, wherein the yttria and alumina sol mixed solution is obtained by dissolving the yttria powder in an acidic solution and then adding an alumina sol. 제1항에 있어서, 상기 하소는 유기물과 수분을 제거할 수 있는 온도범위인 400 - 700℃에서 행해지는 것을 특징으로 하는 안정화 지르코니아 소결체의 제조방법.The method of claim 1, wherein the calcination is carried out at a temperature range from 400 to 700 ° C to remove organic matter and water.
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