KR20050062667A - Mullite based under-floor heating panel using high alumina shale - Google Patents
Mullite based under-floor heating panel using high alumina shale Download PDFInfo
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- KR20050062667A KR20050062667A KR1020030093497A KR20030093497A KR20050062667A KR 20050062667 A KR20050062667 A KR 20050062667A KR 1020030093497 A KR1020030093497 A KR 1020030093497A KR 20030093497 A KR20030093497 A KR 20030093497A KR 20050062667 A KR20050062667 A KR 20050062667A
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- 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
- C04B35/16—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 silicates other than clay
- C04B35/18—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 silicates other than clay rich in aluminium oxide
- C04B35/185—Mullite 3Al2O3-2SiO2
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Abstract
본 발명은 온돌용 세라믹 패널 소지 조성물 및 이를 이용한 온돌용 세라믹 패널 제조 방법에 관한 것이다. 더욱 상세하게는 저가이면서 동시에 고강도, 원적외선 고 방사율을 갖는 온돌 판넬을 제조하기 위하여, 유휴자원인 고알루미나질 반토혈암 중에서 10 wt% 이상의 높은 철분 함량을 갖는 원료를 이용하여 온돌용 세라믹 패널을 제조하는 방법에 관한 것이다. 본 발명에 의하면, Al2O3 함량이 30∼40 wt%, SiO2 함량이 40∼50 wt%, Fe2O3 함량이 10∼16 wt% 인 고알루미나질 반토혈암을 원광을, 원료:물:구석의 비 1 : 1.5 : 1 의 비율로하여 6시간 이상 충분히 분쇄한 후 325 mesh 표준체를 전통시킨 후 50℃에서 건조하여 제조하는 것을 특징으로 하는 온돌용 세라믹 패널 조성물이 제공된다. 또한, 본 발명은 상기 조성물을 프레스 성형 및 압출 성형하여 1100℃에서 1300℃ 범위에서 소성하여, 흡수율 3 % 이하의 고강도, 원적외선 고방사율을 발현 할 수 있는 온돌용 뮬라이트질 세라믹 패널의 제조방법을 제공한다.The present invention relates to an ondol ceramic panel holding composition and a method for producing an ondol ceramic panel using the same. More specifically, in order to manufacture an ondol panel having a low cost, high strength, and far-infrared high emissivity, an ondol ceramic panel is manufactured by using a raw material having a high iron content of 10 wt% or more in the high alumina alumina shale, which is an idle resource. It is about a method. According to the present invention, ore is used as a raw material for high alumina alumina shale with an Al 2 O 3 content of 30 to 40 wt%, an SiO 2 content of 40 to 50 wt%, and a Fe 2 O 3 content of 10 to 16 wt%. There is provided a ceramic panel composition for ondol, which is prepared by pulverizing at least 6 hours in a ratio of water: corner ratio of 1: 1.5: 1 and then preparing a 325 mesh standard and drying at 50 ° C. In another aspect, the present invention provides a method for producing a mullite-like ceramic panel for ondol which can express a high strength, far-infrared high emissivity of 3% or less absorption by baking in the range of 1100 ℃ to 1300 ℃ by press molding and extrusion molding the composition. do.
Description
본 발명은 온돌용 세라믹 패널 소지 조성물 및 이를 이용한 온돌용 세라믹 패널 제조 방법에 관한 것이다. 한국 내 주거 환경의 변화에 의해 건축분야 온돌 관련 법규들이 강화되면서 품질이 유수한 온돌 소재의 개발의 필요성으로 인해 국내 건식 온돌 시장의 시장규모가 점차 확대되는 추세에 있으며, 일본, 중국, 북유럽 등 세계시장 또한 비약적인 증가추세에 있다. 보다 구체적으로는, 저가이면서 동시에 고강도, 원적외선 고 방사율을 갖는 온돌 판넬을 제조하기 위하여, 유휴자원인 고 알루미나질 반토혈암 중에서 10 wt% 이상의 높은 철분 함량을 갖는 원료를 이용하여 온돌용 세라믹 패널을 제조하는 방법에 관한 것이다. The present invention relates to an ondol ceramic panel holding composition and a method for producing an ondol ceramic panel using the same. As the ondol-related regulations in the construction sector are strengthened due to changes in the residential environment in Korea, the market size of the domestic dry ondol market is gradually increasing due to the need for the development of high quality ondol materials, and the global market such as Japan, China and Northern Europe. It is also on the rise. More specifically, in order to manufacture ondol panels having low cost, high strength, and far-infrared high emissivity, an ondol ceramic panel is manufactured using a raw material having a high iron content of 10 wt% or more in high alumina alumina shale, which is an idle resource. It is about how to.
따라서 본 발명에서는 철분 함량 10 % 이상의 반토혈암을 원료로하는 온돌용 세라믹 패널 조성물을 및 이를 이용한 고강도, 원적외선 고방사율 온돌용 세라믹 패널 제조방법을 제공하는 것을 목적으로 하고 있다. 본 발명자는 고 알루미나질 반토혈암을 습식 볼밀하여, 325 mesh 표준체를 전통 시킨 원료를 성형하여, 1200℃ 부근에서 소성 할 경우, 소성 도중에 생성되는 뮬라이트의 상의 생성에 의하여 고강도화가 가능 할 뿐만 아니라, 원적외선 고 방사율 나타낸다는 사실을 알게되어 본 발명을 완성하게 되는 것이다. Therefore, an object of the present invention is to provide a high-strength, far-infrared high-emissivity ondol ceramic panel manufacturing method using the ondol ceramic panel composition having an alumina shale of iron content of 10% or more and the same. The present inventors wet ball mill high alumina alumina shale, and shape a raw material having a 325 mesh standard, and when fired at around 1200 ° C., not only can the strength be increased by the generation of the mullite phase generated during the firing, but also far infrared rays The fact that it shows a high emissivity is to complete the present invention.
그러므로 본 발명에 의하면, Al2O3 함량이 30 ~ 40 wt%, SiO2 함량이 40 ~ 50 wt% Fe2O3 함량이 10 ~ 16 wt% 인 고알루미나질 반토혈암을 원광을, 원료:물:구석의 비 1 : 1.5 : 1 의 비율로하여 6시간 이상 충분히 분쇄한 후 325 mesh 표준체를 전통시킨 것을 특징으로 하는 세라믹 패널 소지 조성물이 제공된다. 또한, 본 발명은 상기의 원료를 프레스성형 및 압출성형하여 얻은 성형체를 1100℃에서 1300℃ 범위에서 소성하여 제조하는 것을 특징으로 하는 온돌용 세라믹 패널 제조 방법을 제공한다.Therefore, according to the present invention, ore is used as a raw material for high alumina alumina shale with an Al 2 O 3 content of 30 to 40 wt%, an SiO 2 content of 40 to 50 wt%, and a Fe 2 O 3 content of 10 to 16 wt%. Provided is a ceramic panel holding composition characterized in that the 325 mesh standard is traditionally pulverized after at least 6 hours in a water: corner ratio of 1: 1.5: 1. In another aspect, the present invention provides a method for producing an on-dol ceramic panel, characterized in that the molded product obtained by pressing and extrusion molding the raw material is produced by firing in the range of 1100 ℃ to 1300 ℃.
이하, 본 발명을 보다 상세하게 설명하기로 한다. 본 발명의 세라믹 패널 소지 조성물은 고 알루미나질 반토혈암으로서, 철분함량이 10 wt% 이상으로 높기 때문에 유휴자원으로서 저가로 확보가능한 원료이다. 주요산지는 전라남도(화순), 강원도(태백, 장성, 정선), 충청북도(단양) 등이다. Hereinafter, the present invention will be described in more detail. The ceramic panel holding composition of the present invention is a high alumina alumina shale, and is a raw material that can be secured at low cost as an idle resource because the iron content is high as 10 wt% or more. The main mountain ranges are Jeollanam-do (Hwasun), Gangwon-do (Taebaek, Jangseong, Jeongseon), and Chungcheongbuk-do (Danyang).
[표 1]에 본 발명의 세라믹 패널 소지 조성물을 구성하는 대표적인 원료로서 세림 대리석 광산(강원도 태백시 장성동 2-3 번지에 소재) 산출의 고 알루미나질 반토혈암의 성분 원소를 XRF 로 분석한 결과를 제시하였다. 단 본 발명은 상기의 세림 대리석 광산 산출의 반토혈암에 한정되지 않으며, 반토혈암 중에서 알루미나 함량이 30 ~ 36 wt%, 철분 함량이 10 ~ 15 wt% 범위의 점토를 모두 포함한다.Table 1 shows the results of XRF analysis of the constituent elements of high alumina alumina shale from the calculation of Serim Marble Mine (2-3, Jangseong-dong, Taebaek-si, Gangwon-do) as a representative raw material constituting the ceramic panel holding composition of the present invention. It was. However, the present invention is not limited to the alumina shale of the serim marble mine output, and includes all clays in the alumina content of 30 to 36 wt% and iron content of 10 to 15 wt% in the alumina shale.
[표 1] 세림 대리석광산 산출 반토 혈암 성분 (XRF 분석결과)[Table 1] Serim Marble Mine Output Alumina Shale Components (XRF Analysis)
( 단위:%) ( unit:%)
[표 1]의 XRF 분석 결과 본 발명을 구성하는 반토혈암은 약 36 wt % 의 높은 Al2O3 함량을 나타내었으며, Fe2O3의 함량 역시 약 16 wt % 정도로 높게 나타났다. 이러한 조성 범위를 갖는 반토혈암은 적당한 열처리 온도에서 뮬라이트질 소지 제조가 가능하다고 판단되었다. 본 발명에서 사용되는 반토혈암은 철분 함량이 매우 높기 때문에 고온에서는 시편이 bloating 현상이 발생할 가능성이 예상되었으며, 또한 철분 함량이 매우 높기 때문에 이 철분을 제거하기 보다는 철분에 의한 갈색계통의 색소지로 개발하는 것이 유리하다고 판단되었다. 본 발명에서 사용되는 반토혈암 원광을 XRD로 상분석한 결과, 홍점토를 구성하는 주요 결정상은 kaolinite, pyrophyllite, α-quartz 이었으며, hematite의 피크도 관찰되었다. 본 발명에서 사용되는 반토혈암은 소성시 mullite 의 생성에 의한 강도 증가를 기대 할 수 있다. XRD 상분석 결과에 의하면 mullite 상의 생성은 1200℃ 부근에서 시작되지만 α-quartz 등의 peak가 사라지기 위해서는 1200℃ 이상의 소성온도가 요구됨을 알 수 있다. 본 발명에서 사용되는 반토혈암을 1150℃ ~ 1300℃ 사이에서 소성하여 제조한 시편의 파단면을 HF 용액으로 에칭한 뒤 주사전자현미경으로 으로 분석하면, 1200℃ ~ 1250℃ 범위에서 침상의 뮬라이트가 interlocking 된 구조를 확인 할 수 있으며, 이 때문에 강도 증가가 예상되는 것이다. 또한 1250℃ 이상에서는 소성시 생성되는 액상의 양이 증가하여 뮬라이트의 입자가 과대 성장하는 것이다.As a result of XRF analysis of Table 1, the alumina shale constituting the present invention showed high Al 2 O 3 content of about 36 wt%, and the content of Fe 2 O 3 was also high as about 16 wt%. It was determined that alumina shale having such a composition range could be prepared for mullite material at an appropriate heat treatment temperature. Since the alumina shale used in the present invention has a very high iron content, the specimen may be bloating at a high temperature, and since the iron content is very high, it is developed as a brown color paper by iron rather than iron removal. It was judged to be advantageous. As a result of phase analysis of the alumina shale ore used in the present invention by XRD, the main crystal phases of red clay were kaolinite, pyrophyllite and α-quartz, and peaks of hematite were also observed. Alumina shale used in the present invention can be expected to increase the strength due to the production of mullite during firing. According to the XRD phase analysis results, the mullite phase is produced around 1200 ° C., but the firing temperature is required to be 1200 ° C. or more in order for the peak of α-quartz and the like to disappear. When the fracture surface of the specimen prepared by calcining the alumina shale used in the present invention between 1150 ℃ and 1300 ℃ is etched with HF solution and analyzed by scanning electron microscope, needle-shaped mullite interlocking in the 1200 ℃ ~ 1250 ℃ range The structure can be identified, which is why the increase in strength is expected. In addition, at 1250 ° C. or more, the amount of the liquid phase generated during firing increases, causing the mullite particles to grow excessively.
본 발명의 조성물로 구성된 세라믹 패널의 소성온도에 따른 물리적 특성을 살펴보면, 1140℃ 부근부터 흡수율이 1% 이하로 떨어짐이 확인되었으며, 1200℃ 부근까지는 소성이 계속 진행되어 수축률이 증가하며, 흡수율이 감소하는 경향을 나타내었다. 꺾임강도 역시 이러한 경향을 반영하고 있으며 1200℃에서 소성하였을 때 894 ㎏f/㎠ 의 최고 값을 나타내었다. 1200℃ 이상에서는 흡수율이 서서히 증가하며, 수축률이 줄어드는 현상이 발생함과 동시에, 꺾임강도도 감소하기 시작하였다. 이러한 현상은 1200℃ 이상에서는 본 발명에서 사용되는 조성물에 존재하는 다량의 산화철 성분들이 Fe2O3에서 FeO 상태로 전이하고자 함에 따라 잉여의 산소를 가스 형태로 서서히 방출하게 되어 시편에 bloating 현상이 발생한 것으로 판단된다. 따라서 본 발명의 조성물을 이용하여 온돌용 세라믹 패널을 제조하기 위해서는 1200℃ 에서 소성 하는 것이 최적이라고 판단되는 것이다.Looking at the physical properties according to the firing temperature of the ceramic panel composed of the composition of the present invention, it was confirmed that the absorption rate drops to less than 1% from around 1140 ℃, the firing continues up to around 1200 ℃ to increase the shrinkage rate, the absorption rate is reduced Showed a tendency to. The bending strength also reflected this tendency and showed the highest value of 894 kgf / ㎠ when fired at 1200 ° C. Above 1200 ° C, the absorption rate gradually increased, shrinkage was reduced, and bending strength also began to decrease. This phenomenon occurs at a temperature of 1200 ° C. or more, as a large amount of iron oxide components present in the composition used in the present invention attempts to transition from Fe 2 O 3 to FeO state, releasing excess oxygen in a gaseous form, thereby causing bloating. It seems to be. Therefore, in order to manufacture an ondol ceramic panel using the composition of this invention, it is judged that baking at 1200 degreeC is optimal.
일반적으로 세라믹스의 원적외선 방사특성에 관해서는 많은 연구보고와 결과들이 있으며, SiO2나 Al2O3를 주성분으로 하는 뮬라이트, 코디어라이트 지르콘, 스포듀민 계 및 화학조성이 유사한 계가 우수한 원적외선 방사체의 방사특성을 갖는 것으로 알려져 있다. 본 발명에서 사용되는 조성물의 경우 높은 원적이선 방사율이 기대되는데 1200℃ 소성 시편의 경우 40℃에서 0.930 의 매우 높은 원적외선 방사율을 얻을 수 있었다. 이상 설명 한 바와 같은 본 발명의 특징 및 기타 장점은 후술되는 실시예로부터 보다 명백하게 될 것이다. 단, 본 발명은 하기 실시예로 한정되는 것은 아니다.In general, there are many reports and results regarding the far-infrared radiation characteristics of ceramics, and the emission of far-infrared radiators with excellent mullite, cordierite zircon, spodumene, and similar chemical compositions, mainly composed of SiO 2 or Al 2 O 3 It is known to have characteristics. In the case of the composition used in the present invention, high far-infrared emissivity is expected, but in the case of 1200 ° C fired specimens, a very high far-infrared emissivity of 0.930 was obtained at 40 ° C. Features and other advantages of the present invention as described above will become more apparent from the following examples. However, the present invention is not limited to the following examples.
< 실시예 1><Example 1>
세림 대리석 광산(강원도 태백시 장성동 2-3 번지에 소재) 산출의 고알루미나질 반토혈암 (조성은 표 1 참조) 을 시료 : 물 : 구석 비 1 : 1.5 : 1 로 하여 24시간 습식 분쇄 한 후 325 mesh 표준체를 전통 시킨 후 50℃에서 건조하여 원료를 제조하였다. 이것을 Ø 36.0㎜의 금형에 100 ㎏f/㎠ 의 압력으로 성형하였다. 시편의 소성은 산화분위기에서 소성온도 1,120℃, 1,140℃, 1,160℃, 1,180℃, 1200℃, 1230℃, 1250℃ 및 1280℃ 에서 각각 소성하였으며, 수축률, 흡수율, 꺽임강도를 평가하여 그 결과를 [표 2]에 나타내었다. 또한 1200℃ 소성 시편의 원적외선 방사율 (40℃)을 측정하여, 비교 예로서 동일 조건에서 측정한 Al2O3 판의 원적외선 방사율과 함께 [표 3] 에 결과를 정리하였다.High-alumina alumina shale (composition, see Table 1) of the Serim Marble Mine (2-3, Jangseong-dong, Taebaek-si, Gangwon-do) was subjected to wet pulverization for 24 hours with a sample: water: corner ratio of 1: 1.5: 1 and 325 mesh. After preparing the standard, dried at 50 ℃ to prepare a raw material. This was molded into a mold of 36.0 mm at a pressure of 100 kgf / cm 2. The specimens were fired at oxidizing atmosphere at 1,120 ℃, 1,140 ℃, 1,160 ℃, 1,180 ℃, 1200 ℃, 1230 ℃, 1250 ℃ and 1280 ℃, and evaluated for shrinkage, absorption and bending strength. Table 2]. In addition, the far-infrared emissivity (40 ° C) of the 1200 ° C fired specimens was measured, and the results are summarized in Table 3 together with the far-infrared emissivity of the Al 2 O 3 plate measured under the same conditions as a comparative example.
[ 표 2] 소성 온도에 따른 물리적 특성[Table 2] Physical Properties According to Firing Temperature
[표 3] 고알루미나질 반토혈암 소지조합 세라믹스의 원적외선 방사율 [Table 3] Far-infrared emissivity of high alumina alumina shale combination ceramics
이상에서 상술한 바와 같이 본 발명은, 철분 함량이 높아 용도 개발이 제한적이었던 고 알루미나질 반토혈암의 새로운 용도개발이라는 효과를 갖는다. 고강도이고 심미성이 뛰어날 뿐만 아니라, 원적외선 고방사율 특성을 갖는 소재를 개발하였다. 본 발명을 상업화한다면, 온돌판넬은 물론, 천연대리석을 대체 할 수 있는 심미성 소재, 인체 및 환경친화성 건축소재로서 개발 가능성이 크다고 할 수 있다. 또한 국내 원적외선 목욕 문화시설에 및 주택 주거시설 등 온돌문화 조성에 활용될 수 있다.As described above, the present invention has the effect of developing a new use of high alumina alumina, which has a high iron content and limited use in development. In addition to high strength and aesthetics, a material with far-infrared high emissivity properties has been developed. If you commercialize the present invention, it can be said that the development potential as aesthetic material, human body and environmentally friendly building material that can replace natural marble as well as ondol panel. In addition, it can be used to create an ondol culture such as domestic far-infrared bath culture facilities and residential housing facilities.
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