KR101364484B1 - Method of preparing porous silicon nitride ceramics and porous silicon nitride ceramics thereof - Google Patents
Method of preparing porous silicon nitride ceramics and porous silicon nitride ceramics thereof Download PDFInfo
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Abstract
다공성 질화규소 요업체 제조방법 및 그에 의한 다공성 질화규소 요업체가 개시된다. 본 발명은 (a) 22 중량% 내지 30 중량%의 Si3N4 와 70 중량% 내지 78 중량%의 Y2O3를 혼합하여 저융점 조성분말을 제조하는 단계, (b) 저융점 조성분말을 구상으로 성형하는 단계, (c) 구상으로 성형된 구상화 저융점 조성분말을 열처리하여 구상화 저융점 미립자를 제조하는 단계, (d) 구상화 저융점 미립자를 Si3N4 및 Y2O3를 포함하는 혼합분말에 첨가하여 구상화 저융점 미립자 포함 혼합분말을 제조하는 단계, 및 (e) 구상화 저융점 미립자 포함 혼합분말을 불활성 분위기 중에서 소결하는 단계를 통해 구현된다. 본 발명에 의하면, 균일한 크기의 미세한 기공이 형성되어 있어 가볍고 내열성이 우수한 다공성 질화규소 요업체를 제조할 수 있게 된다.Disclosed are a method for producing a porous silicon nitride agent and a porous silicon nitride agent thereby. The present invention comprises the steps of (a) mixing 22 wt% to 30 wt% of Si 3 N 4 and 70 wt% to 78 wt% of Y 2 O 3 to prepare a low melting point composition powder, (b) a low melting point composition powder Forming spherical particles, (c) heat-treating spheroidized low melting point composition powders to form spherical low melting point particles, and (d) Si 3 N 4 and Y 2 O 3 Adding to the mixed powder to prepare a mixed powder containing spherical low melting point fine particles, and (e) sintering the mixed powder containing spherical low melting point fine particles in an inert atmosphere. According to the present invention, fine pores of uniform size are formed, thereby making it possible to manufacture a porous silicon nitride insulator having excellent light and heat resistance.
질화규소, 요업체, 저융점, 다공성, 산화이트륨 Silicon Nitride, Ceramics, Low Melting Point, Porous, Yttrium
Description
본 발명은 다공성 질화규소 요업체 제조방법 및 그에 의한 다공성 질화규소 요업체에 관한 것으로, 더욱 상세하게는 가벼우면서 수 밀리미터 크기의 미세 기공이 균일하게 형성되어 있는 다공성 질화규소 요업체 제조방법 및 그에 의한 다공성 질화규소 요업체에 관한 것이다.The present invention relates to a method for manufacturing a porous silicon nitride main body and a porous silicon nitride main body, and more particularly, a method for manufacturing a porous silicon nitride main body and a porous silicon nitride key It's about the company.
질화 규소 요업체(ceramics)는 질화규소를 기본으로 하고 여러 산화물인 질화물이 소결제조로 첨가되어 제조되며, 이러한 질화 규소 요업체는 비중이 낮고, 경도가 우수하며 화학적 안정성 및 내열성이 우수한 특징을 가진다.Silicon nitride carriers (ceramics) are based on silicon nitride and manufactured by sintering of various oxide nitrides. These silicon nitride carriers have low specific gravity, excellent hardness, excellent chemical stability and heat resistance.
질화규소 요업체에는 일반적으로 Si3N4에 마그네시아(MgO), 알루미나(Al2O3) 등을 보조제로서 첨가한 후, 이러한 혼합물을 소결하여 제조되는 β-Si3N4, 알루미나와 질화알루미늄, 또는 실리카와 질화알루미늄을 특정한 비율로 첨가하여 β-Si3N4의 결정 구조를 유지하면서 Si과 Ni이 각각 Al과 O로 치환된 β-사이알 론(sialon), 또한 기본적으로 α-Si3N4의 결정 구조를 유지하면서 Si와 N이 각각 Al과 O로 치환된 α-사이알론이 있다.Silicon nitride requires companies typically Si 3 N 4 magnesia (MgO), alumina (Al 2 O 3), etc., and then added as an auxiliary agent, β-Si 3 which is prepared by sintering this mixture N 4, alumina and aluminum nitride in, Or β-sialon in which Si and Ni are substituted with Al and O while maintaining the crystal structure of β-Si 3 N 4 by adding silica and aluminum nitride in a specific ratio, and basically α-Si 3 There is an α-sialon in which Si and N are substituted with Al and O while maintaining the crystal structure of N 4 .
이러한 질화규소 요업체와 더불어 질화규소와 실리카가 몰비로서 1:1로 고용되어 형성되는 질화규소 요업체가 존재하며, 이러한 질화규소 요업체는 주로 고온내화재료로서 이용되고 있다.In addition to these silicon nitride components, there are silicon nitride components in which silicon nitride and silica are employed in a molar ratio of 1: 1, and these silicon nitride components are mainly used as high temperature refractory materials.
한편, 이와 같이 다양한 원료 분말이 혼합된 질화규소 요업체에는, 질화규소 및 다른 소결 조제가 혼합, 성형, 소결되는 과정에서 발달한 액상이 치밀화를 촉진한 후 점차 반응 생성된 입자에 고용되어 최종적으로 고상 및 불규칙한 형태의 기공이 남게 된다는 문제점이 있다.On the other hand, in the silicon nitride main material in which various raw material powders are mixed, the liquid phase developed in the process of mixing, forming, and sintering silicon nitride and other sintering aids promotes densification, and is then employed in particles that are gradually reacted to produce solid phase and There is a problem that pores of irregular shape remain.
이러한 잔류 기공의 형태를 제어하기 위하여, 최종적으로 탄화규소 및 질화규소로 분해되는 세라믹 전구체(ceramic precursor)를 첨가하여 요업체를 제조하는 방법(미국 특허 제 5,643,987호)이 제안되었으나, 이러한 경우에 발달되는 기공은 수십 옹스트롬의 극미세 기공으로서, 내화물에 요구되는 수 밀리미터 크기의 기공 발달에는 적합하지 아니하다.In order to control the morphology of these residual pores, a method of preparing a urinary agent by adding a ceramic precursor which is finally decomposed into silicon carbide and silicon nitride (US Pat. No. 5,643,987) has been proposed. The pores are micropores of tens of angstroms and are not suitable for the development of pores of the millimeter size required for refractory materials.
따라서, 본 발명의 목적은, 가벼우면서 수 밀리미터 크기의 미세 기공이 균일하게 형성되어 있는 다공성 질화규소 요업체 제조방법 및 그에 의한 다공성 질화규소 요업체를 제공함에 있다.Accordingly, it is an object of the present invention to provide a porous silicon nitride warehousing method and a porous silicon nitride warehousing process, in which light micropores having a size of several millimeters are formed uniformly.
상기 목적을 달성하기 위한 본 발명에 따른 다공성 질화규소 요업체 제조방법은 (a) 22 중량% 내지 30 중량%의 Si3N4 와 70 중량% 내지 78 중량%의 Y2O3를 혼합하여 저융점 조성분말을 제조하는 단계, (b) 상기 제조된 저융점 조성분말을 구상으로 성형하는 단계, (c) 상기 구상으로 성형된 구상화 저융점 조성분말을 열처리하여 구상화 저융점 미립자를 제조하는 단계, (d) 상기 제조된 구상화 저융점 미립자를 Si3N4 및 Y2O3를 포함하는 혼합분말에 첨가하여 구상화 저융점 미립자 포함 혼합분말을 제조하는 단계, 및 (e) 상기 제조된 구상화 저융점 미립자 포함 혼합분말을 불활성 분위기 중에서 소결하는 단계를 포함한다.Porous silicon nitride manufacturing method according to the present invention for achieving the above object is (a) low melting point by mixing 22% to 30% by weight of Si 3 N 4 and 70% to 78% by weight of Y 2 O 3 Preparing a composition powder, (b) forming the prepared low melting composition powder into a spherical shape, (c) heat-treating the spheroidized low melting composition powder formed into a spherical shape to prepare spheroidized low melting point fine particles, ( d) adding the prepared spheroidized low melting point fine particles to the mixed powder containing Si 3 N 4 and Y 2 O 3 to prepare a mixed powder including spheroidized low melting point fine particles, and (e) the spheroidized low melting point fine particles prepared above. Sintering the containing mixed powder in an inert atmosphere.
바람직하게는, 상기 (c) 단계는, 상기 구상으로 성형된 구상화 저융점 조성분말을 400℃ 내지 600℃에서 0.5시간 내지 2시간 동안 열처리하는 것을 특징으로 한다. Preferably, the step (c) is characterized in that the spheroidized low melting point composition powder is formed into a heat treatment at 400 ℃ to 600 ℃ for 0.5 hours to 2 hours.
또한, 상기 (c) 단계에서 제조된 상기 구상화 저융점 미립자의 크기는 0.01mm 내지 1.0mm 인 것을 특징으로 한다. In addition, the size of the spherical low melting point fine particles prepared in step (c) is characterized in that 0.01mm to 1.0mm.
또한, 상기 (d) 단계에서, 상기 Si3N4 및 Y2O3를 포함하는 혼합분말은 38.3 중량%의 Si3N4 와 61.7 중량%의 Y2O3를 포함하는 것을 특징으로 한다. In addition, in the step (d), the mixed powder comprising Si 3 N 4 and Y 2 O 3 is characterized in that it comprises 38.3% by weight of Si 3 N 4 and 61.7% by weight of Y 2 O 3 .
또한, 상기 (d) 단계는, 상기 Si3N4 및 Y2O3를 포함하는 혼합분말에 상기 구상화 저융점 미립자를 5 중량% 내지 10 중량% 가 되도록 첨가하는 것을 특징으로 한다. In addition, the step (d) is characterized in that to add the spherical low melting point fine particles to 5 to 10% by weight to the mixed powder containing the Si 3 N 4 and Y 2 O 3 .
또한, 상기 (e) 단계는, 상기 구상화 저융점 미립자 포함 혼합분말을 1650℃ 내지 1750℃에서 1시간 내지 2시간 동안 소결하는 것을 특징으로 한다. In addition, the step (e) is characterized in that for sintering the mixed powder containing the spherical low melting point fine particles at 1650 ℃ to 1750 ℃ for 1 hour to 2 hours.
또한, 상기 구상화 저융점 미립자를 첨가하여 제조된 다공성 질화규소 요업체에는 0.1㎜ 내지 0.5㎜ 크기의 구형 기공이 생성되는 것을 특징으로 한다. In addition, the porous silicon nitride ingot manufactured by adding the spheroidized low melting point fine particles is characterized in that the spherical pores of 0.1mm to 0.5mm size is produced.
한편, 본 발명에 따른 다공성 질화규소 요업체는 상기 다공성 질화규소 요업체 제조방법에 의해 제조되는 것을 특징으로 한다.On the other hand, the porous silicon nitride main company according to the invention is characterized in that it is manufactured by the method for producing a porous silicon nitride main company.
본 발명에 따르면, 구상화 저융점 미립자를 첨가하여 소결 처리함으로써, 균일한 크기의 미세한 기공이 형성되어 있어 가볍고 내열성이 우수한 다공성 질화규소 요업체를 제조할 수 있게 된다.According to the present invention, by adding the spherical low melting point fine particles and sintering, fine pores of uniform size are formed, thereby making it possible to manufacture a porous silicon nitride main body having excellent light and heat resistance.
이하에서는 도면을 참조하여 본 발명을 보다 상세하게 설명한다. 도면들 중 동일한 구성요소들은 가능한 한 어느 곳에서든지 동일한 부호들로 나타내고 있음에 유의해야 한다. 또한 본 발명의 요지를 불필요하게 흐릴 수 있는 공지 기능 및 구성에 대한 상세한 설명은 생략한다. Hereinafter, the present invention will be described in detail with reference to the drawings. It is to be noted that the same elements among the drawings are denoted by the same reference numerals whenever possible. In the following description, well-known functions or constructions are not described in detail since they would obscure the invention in unnecessary detail.
도 1은 본 발명에 따른 다공성 질화규소 요업체 제조방법의 공정을 나타내는 절차 흐름도이다.1 is a procedure flow diagram illustrating a process of a method for producing a porous silicon nitride major company according to the present invention.
도 1을 참조하여, 본 발명에 따른 다공성 질화규소 요업체 제조방법의 공정을 살펴보면, 본 발명에 따른 다공성 질화규소 요업체를 제조하기 위해서는, 먼저, Si3N4 와 Y2O3 를 혼합하여, 22 중량% 내지 30 중량%의 Si3N4 와 70 중량% 내지 78 중량%의 Y2O3 를 포함하는 저융점 조성분말을 제조한다(S100). 한편, 본 발명을 실시함에 있어서는, 특히 26 중량%의 Si3N4 와 74 중량%의 Y2O3 를 포함하는 저융점 조성분말을 제조하는 것이 바람직하다.Referring to Figure 1, looking at the process of manufacturing a porous silicon nitride in accordance with the present invention, in order to prepare a porous silicon nitride in accordance with the present invention, first, by mixing Si 3 N 4 and Y 2 O 3 , 22 A low melting point composition powder including Si 3 N 4 in an amount of 30 wt% to 70 wt% and Y 2 O 3 in an amount of 70 wt% to 78 wt% is prepared (S100). On the other hand, in carrying out the present invention, it is particularly preferable to prepare a low melting point composition powder comprising 26% by weight of Si 3 N 4 and 74% by weight of Y 2 O 3 .
이와 같은 22 중량% 내지 30 중량%의 Si3N4 와 70 중량% 내지 78 중량%의 Y2O3 를 포함하는 저융점 조성은 Y2O3 및 Si3N4로 이루어진 계가 1650℃에서 액상을 발달시키고 그 액상이 Y2O3 및 Y2Si3O3N4 와 상평형을 이루는 조성으로서, 이 조성 범위를 벗어날 경우, 본 발명에서 목적하지 않는 고상 입자가 발달하여 구형 기공 발달을 방해할 수 있다.The low melting point composition comprising 22 wt% to 30 wt% of Si 3 N 4 and 70 wt% to 78 wt% of Y 2 O 3 is a system composed of Y 2 O 3 and Si 3 N 4 in a liquid phase at 1650 ° C. And the liquid phase is in phase equilibrium with Y 2 O 3 and Y 2 Si 3 O 3 N 4 , when outside the composition range, solid particles, which are not intended in the present invention, develop to hinder the development of spherical pores. can do.
또한, 액상조성 영역은 좁기 때문에 Si3N4가 22 중량% 미만 또는 30 중량% 초과일 경우, 즉 Y2O3가 70 중량% 미만 또는 78 중량% 초과일 경우에는 본 발명이 목적하는 액상 이외의 다른 상이 발달하거나 미반응 원료입자가 잔존하여 발명이 목적하는 기공형성 효과를 해치게 되는 것이다.In addition, since the liquid composition region is narrow, when Si 3 N 4 is less than 22% or more than 30% by weight, that is, when Y 2 O 3 is less than 70% or more than 78% by weight, the liquid phase other than the object of the present invention is used. Other phases of the development or unreacted raw material particles remain to harm the intended pore-forming effect of the invention.
그 다음, 22 중량% 내지 30 중량%의 Si3N4 와 70 중량% 내지 78 중량%의 Y2O3 를 포함하는 저융점 조성분말을 구상으로 성형한다(S110). 한편, 저융점 조성분말을 구상으로 성형하는 구상화 공정에서는 V형 혼합기와 같은 진동 혼합기에 투입하고, 진동 혼합기를 돌려가면서 혼합하는 방법을 사용하는 것이 바람직할 것이다.Next, a low melting composition powder containing 22 wt% to 30 wt% Si 3 N 4 and 70 wt% to 78 wt% Y 2 O 3 is formed into a sphere (S110). On the other hand, in the spheroidizing process of forming a low melting point composition powder into a spherical shape, it may be preferable to use a method of mixing the mixture while turning the vibrating mixer such as a V-type mixer.
그 다음, 구상으로 성형된 생성물을 400℃ 내지 600℃에서 0.5시간 내지 2시간 동안 열처리하여 기공형성체 역할을 하는 구상화 저융점 미립자를 제조한다(S120). 여기서 구상의 생성물을 400℃ 내지 600℃에서 열처리 하는 것은 일종의 가소결을 실시하여 이후에 이어지는 공정 중 파손되거나 변형되어 구상형태가 상실되는 것을 방지하기 위한 것으로, 400℃ 미만의 온도나 0.5시간 미만의 시간에서는 충분한 강도가 얻어지지 않으며, 600℃ 초과의 온도나 2 시간 초과의 시간은 목적하는 물성을 얻는데 필요한 그 이상의 에너지와 공정시간을 낭비하게 된다. Next, the spherically shaped product is heat-treated at 400 ° C. to 600 ° C. for 0.5 to 2 hours to produce spheroidized low melting fine particles serving as pore-forming bodies (S120). Here, the heat treatment of the spherical product at 400 ℃ to 600 ℃ is a kind of pre-sintering to prevent the loss of spherical shape due to breakage or deformation during the subsequent process, the temperature of less than 400 ℃ or less than 0.5 hours In time, sufficient strength is not obtained, and temperatures above 600 ° C. or more than 2 hours waste additional energy and processing time necessary to obtain the desired properties.
이와 같은 공정으로 제조된 상기 구상화 저융점 미립자의 평균 크기는 통상적으로 0.01mm 내지 1.0mm가 된다. 한편, 본 발명에 따른 다공성 요업체를 일반적인 내화벽돌로 이용하는 경우에는, 구상화 저융점 미립자의 평균 크기는 특히 0.1mm 내지 0.5mm 인 것이 바람직하다. 따라서, 전술한 S120 단계에서 제조된 구상화 저 융점 미립자를 분급하여 용도에 따라 용구되는 소정 크기의 것들을 골라 모으게 된다(S130). The average size of the spherical low melting point fine particles produced by such a process is usually from 0.01mm to 1.0mm. On the other hand, in the case of using the porous ceramics according to the present invention as a general refractory brick, the average size of the spheroidized low melting point fine particles is particularly preferably 0.1mm to 0.5mm. Therefore, the spheroidized low melting point fine particles prepared in step S120 described above are sorted to collect those having a predetermined size according to the use (S130).
한편, 다공성 요업체에 요구되는 기공크기에 따라 저융점 미립자의 크기는 자유로이 조절할 수 있는 것이므로 일반적인 요업공정에 부합되는 한 그 크기는 특별히 한정되지는 않을 것이다.On the other hand, the size of the low melting point fine particles can be freely adjusted according to the pore size required by the porous ceramics manufacturers will not be particularly limited as long as it meets the general ceramic process.
이와 같이 제조 및 분류된 소정 크기의 구상화 저융점 미립자는 이후에 설명할 소결과정에서 질화규소 입자 사이로 침투하여 소결조제로 작용하는 한편 미세한 구형 기공을 형성하게 된다.The spheroidized low melting fine particles of the predetermined size prepared and classified as described above penetrate between the silicon nitride particles in the sintering process to be described later to form a sintering aid and form fine spherical pores.
그 다음, 38.3 중량%의 Si3N4 와 61.7 중량%의 Y2O3를 혼합하여 혼합분말을 제조한다(S140). 이러한 조성은 Y2Si3O3N4 요업체의 조성으로서 전술한 저융점 조성 액상과 상평형을 이루게 된다.Then, 38.3 wt.% Si 3 N 4 61.7 wt% of Y 2 O 3 is mixed to prepare a mixed powder (S140). This composition is Y 2 Si 3 O 3 N 4 As the composition of the urethane maker, it is in phase equilibrium with the above-described low melting point liquid phase liquid.
38.3 중량%의 Si3N4 와 61.7 중량%의 Y2O3를 혼합하여 제조된 혼합분말에 구상화 저융점 미립자를 5 중량% 내지 10 중량%로 첨가하여 구상화 저융점 미립자 포함 혼합분말을 제조한다(S150). 한편, 본 발명을 실시함에 있어서는, 혼합분말 95 중량% 내지 96 중량% 중에 구상화 저융점 미립자 7 중량% 내지 8 중량%를 첨가함으로써, 구상화 저융점 미립자포함 혼합분말을 제조함이 바람직할 것이다.38.3 wt.% Si 3 N 4 Spherical low melting point fine particles are added to the mixed powder prepared by mixing 61.7% by weight of Y 2 O 3 to 5% by weight to 10% by weight to prepare a mixed powder containing spherical low melting point fine particles (S150). On the other hand, in the practice of the present invention, it will be preferable to prepare a mixed powder containing spherical low melting point fine particles by adding 7% to 8% by weight of spherical low melting point fine particles in 95% by weight to 96% by weight mixed powder.
한편, 구상화 저융점 미립자의 사용량이 5 중량% 미만일 경우에는 다공성 질화규소 요업체 제조에 대한 효과가 적고, 구상화 저융점 미립자의 사용량이 10 중량%를 초과할 경우에는 소결 중 발생되는 액상이 많아 입자 재배열 현상이 심화되 어 구형의 기공 형태 유지가 어렵게 된다.On the other hand, when the amount of spheroidized low melting point fine particles is less than 5% by weight, the effect on the manufacture of porous silicon nitride is small, and when the amount of spheroidized low melting point fine particles exceeds 10% by weight, the amount of liquid generated during sintering is high. As the arrangement becomes more severe, it becomes difficult to maintain the spherical pore shape.
이와 같이 제조된 구상화 저융점 미립자 포함 혼합분말을 질소, 더 바람직하게는 아르곤과 같은 불활성 분위기 중에서 1650℃ 내지 1750℃에서 1시간 내지 2시간 동안 소결하여 다공성 질화규소 요업체를 제조하게 된다(S160). The spheroidized low melting point fine particles containing the powder thus prepared are sintered at 1650 ° C. to 1750 ° C. for 1 hour to 2 hours in an inert atmosphere such as nitrogen, and more preferably argon (S160).
한편, 소결 온도가 1650℃ 보다 낮을 경우에는 치밀한 소결체의 제조가 어렵고, 1750℃보다 높을 경우에는 저융점 조성 액상의 휘발이나 Si3N4의 분해로 강도 저하가 심해지는 문제점이 있다. On the other hand, when the sintering temperature is lower than 1650 ° C, it is difficult to manufacture a dense sintered body, and when the sintering temperature is higher than 1750 ° C, there is a problem in that the strength decreases due to volatilization of the low melting point composition liquid or decomposition of Si 3 N 4 .
소결 시간은 소결 온도가 높을수록 짧아지며, 1650℃ 소결 온도에서는 적어도 2시간 이상 가열함으로써 본 발명에서 의도적으로 형성시킨 기공을 제외하면 그 기지가 치밀하고 강한 소결체를 얻을 수 있게 된다.The sintering time becomes shorter as the sintering temperature is higher, and at a sintering temperature of 1650 ° C., at least 2 hours is heated, except for the pores formed intentionally in the present invention, thereby obtaining a compact and strong sintered body.
이러한 소결 공정에서, 저융점 조성 분말이 용융되어 액상이 형성되며, 이렇게 형성된 액상은 Si3N4, Y2O3 및 이들이 반응하여 생성되는 Y2Si3O3N4 입자 사이의 계면에 침투하여 반응을 촉진시키고, 분말 사이의 모세관에 침투되어 치밀화를 촉진하게 된다. 한편, 이와 동시에 저융점 조성의 구상화 미립자가 있던 자리는 빈 공간, 즉 구형의 기공으로 남게 된다.In this sintering process, the low melting composition powder is melted to form a liquid phase, and the liquid phase thus formed penetrates into the interface between Si 3 N 4 , Y 2 O 3 and the Y 2 Si 3 O 3 N 4 particles produced by the reaction thereof. To accelerate the reaction and to penetrate the capillaries between the powders to promote densification. At the same time, the site where the spheroidized microparticles | fine-particles of a low melting point composition existed remains in an empty space, ie, a spherical pore.
따라서, 본 발명에 의해 저융점 조성분말을 구상화하여 첨가함으로써, 질화규소 소결체 제조 공정시 저융점 조성분말이 액상화되어 질화규소 입자 간에 형성되는 모세관에 빨려들어감으로써, 최종적으로는 구형의 기공들이 균일하게 분포된 질화규소 요업체를 얻게 된다.Therefore, by spheroidizing the low melting composition powder according to the present invention, the low melting composition powder is liquefied in the silicon nitride sintered manufacturing process and sucked into the capillary formed between the silicon nitride particles, and finally the spherical pores are uniformly distributed. You get a silicon nitride supplier.
즉, 본 발명에 따른 다공성 질화규소 요업체는 저융점 조성 분말 및 미립자를 먼저 제조하고 이를 소결조제 및 기공형성제로 이용함으로써 제조되는 것이다.That is, the porous silicon nitride carrier according to the present invention is prepared by first preparing a low melting point composition powder and fine particles and using it as a sintering aid and a pore-forming agent.
이하에서는 실시예를 통해 본 발명에 따른 다공성 질화규소 요업체 제조방법을 설명하기로 한다. Hereinafter will be described a porous silicon nitride key material manufacturing method according to the present invention through the examples.
- - 실시예Example 1 - One -
26 중량%의 Si3N4 와 74 중량%의 Y2O3 를 V형 혼합기에 넣고 30분 이상 혼합하여 구상화한다. 이렇게 구상화된 혼합물을 500℃에서 1시간 가량 열처리하여, 구상화 저융점 조성 미립자를 제조한다. 그 다음, 제조된 분말을 분급하여 그 크기가 0.1㎜ 내지 0.5㎜인 것들을 모은다.26 wt% Si 3 N 4 and 74 wt% Y 2 O 3 are added to a V-type mixer and mixed for 30 minutes or more to form a spheroid. The spheroidized mixture was heat-treated at 500 ° C. for 1 hour to produce spheroidized low melting point composition fine particles. Then, the prepared powder is classified and those having a size of 0.1 mm to 0.5 mm are collected.
한편, 38.3 중량%의 Si3N4 와 61.7 중량%의 Y2O3 를 V형 혼합기에 넣고 30분 이상 혼합하여 혼합분말을 제조한다. 그리고 상기 0.1㎜ 내지 0.5㎜의 크기를 갖는 구상화 저융점 미립자 8 중량%를 상기 혼합분말 92 중량%에 첨가하여 혼합하고, 이를 아르곤 분위기 중에서 1700℃로 1시간 소결하여 다공성 질화규소 요업체를 제조한다.Meanwhile, 38.3% by weight of Si 3 N 4 and 61.7% by weight of Y 2 O 3 were added to a V-type mixer and mixed for 30 minutes or more to prepare a mixed powder. And 8% by weight of the spherical low melting point fine particles having a size of 0.1mm to 0.5mm is added to 92% by weight of the mixed powder and mixed, and sintered at 1700 ℃ for 1 hour in argon atmosphere to prepare a porous silicon nitride core.
이와 같이 얻어진 요업체에는 구상화 저융점 미립자에 의한 0.1㎜ 내지 0.5㎜ 크기의 구형 기공이 생성되며 기공율은 약 10%가 된다.The urine obtained in this way produces spherical pores with a size of 0.1 mm to 0.5 mm due to spheroidized low melting point fine particles and the porosity is about 10%.
이상에서는 본 발명의 바람직한 실시예 및 응용예에 대하여 도시하고 설명하였지만, 본 발명은 상술한 특정의 실시예 및 응용예에 한정되지 아니하며, 청구범 위에서 청구하는 본 발명의 요지를 벗어남이 없이 당해 발명이 속하는 기술분야에서 통상의 지식을 가진자에 의해 다양한 변형실시가 가능한 것은 물론이고, 이러한 변형실시들은 본 발명의 기술적 사상이나 전망으로부터 개별적으로 이해되어져서는 안될 것이다.Although the above has been shown and described with respect to preferred embodiments and applications of the present invention, the present invention is not limited to the specific embodiments and applications described above, the invention without departing from the gist of the invention claimed in the claims Various modifications can be made by those skilled in the art, and these modifications should not be individually understood from the technical spirit or the prospect of the present invention.
도 1은 본 발명에 따른 다공성 질화규소 요업체 제조방법의 공정을 나타내는 절차 흐름도이다.1 is a procedure flow diagram illustrating a process of a method for producing a porous silicon nitride major company according to the present invention.
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| US4629707A (en) * | 1986-01-21 | 1986-12-16 | Gte Products Corporation | High strength, low mass porous silicon nitride based articles |
| EP1197253A1 (en) * | 2000-10-13 | 2002-04-17 | Asahi Glass Company Ltd. | Method for producing a silicon nitride filter |
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| US4629707A (en) * | 1986-01-21 | 1986-12-16 | Gte Products Corporation | High strength, low mass porous silicon nitride based articles |
| EP1197253A1 (en) * | 2000-10-13 | 2002-04-17 | Asahi Glass Company Ltd. | Method for producing a silicon nitride filter |
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| KR20090067936A (en) | 2009-06-25 |
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