KR20140031799A - Manufacturing apparatus for realizing in-line system of material nitride for led red phosphor, and method thereof - Google Patents

Manufacturing apparatus for realizing in-line system of material nitride for led red phosphor, and method thereof Download PDF

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KR20140031799A
KR20140031799A KR1020130105368A KR20130105368A KR20140031799A KR 20140031799 A KR20140031799 A KR 20140031799A KR 1020130105368 A KR1020130105368 A KR 1020130105368A KR 20130105368 A KR20130105368 A KR 20130105368A KR 20140031799 A KR20140031799 A KR 20140031799A
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raw material
nitride
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material nitride
red phosphor
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KR101564625B1 (en
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윤원규
박주현
김경용
황병진
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희성금속 주식회사
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    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
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Abstract

The present invention relates to a method for manufacturing metal material used for manufacturing LED red phosphor by nitrification, and maximizing the nitrogen content and minimizing the contamination of oxygen by in-line integrating the nitrification and grinding process. And the method comprises the steps of nitrifying the metal material and mechanically grinding the nitrated nitride of material. [Reference numerals] (AA) Nitrogen input; (BB) Nitrogen emission

Description

ＬＥＤ 적색형광체용 원료질화물 Ｉｎ-ｌｉｎｅ화 제조장치 및 방법{Manufacturing apparatus for realizing in-line system of material nitride for LED red phosphor, and method thereof}Manufacturing apparatus for realizing in-line system of material nitride for LED red phosphor, and method

본 발명은 LED의 핵심소재인 형광체 중 적색형광체의 제조에 이용되는 금속원료를 질화 반응시켜 제조하는 방법으로서 질화반응과 분쇄공정을 In-line일체화하여 제조하는 것을 특징으로 하는 제조장치 및 방법에 관한 것이다. 상세하게는 금속원료에 일정한 양과 시간으로 질소가스 또는 질소수소 혼합가스를 사용하여 일정한 온도로 질화 시킴으로써 질소함량은 최대로 하며 산소오염을 최소화하는 제조장치 및 방법에 관한 것이다.The present invention relates to a method for producing a nitriding reaction of a metal raw material used in the manufacture of a red phosphor among the phosphors, which is a key material of LED, and to a manufacturing apparatus and method characterized in that the nitriding reaction and the pulverization process are manufactured by in-line integration. will be. Specifically, the present invention relates to a manufacturing apparatus and a method for maximizing nitrogen content and minimizing oxygen pollution by nitriding a metal material at a constant temperature using nitrogen gas or nitrogen-hydrogen mixed gas in a constant amount and time.

최근 들어, LED TV 및 조명 시장이 점차 증가함에 따라 LED용 적색형광체의 수요가 늘어나고 있으며 LED용 적색형광체 제조를 위하여 원료질화물의 수요가 증대되고 있다. 그러나 원료질화물은 산소에 접촉 시 제품이 급격하게 산화가 되는 문제가 있다. 그래서 대기에 방치할 경우 단시간에 산화가 되므로 제품 제조 시 질소분위기의 환경에서 작업이 이루어져야 한다.Recently, as the LED TV and lighting market gradually increases, the demand for red phosphors for LEDs is increasing, and the demand for raw material nitride is increasing for the manufacture of red phosphors for LEDs. However, the raw material nitride has a problem that the product is rapidly oxidized when contacted with oxygen. Therefore, when it is left in the atmosphere, since it oxidizes in a short time, work should be done in the environment of nitrogen atmosphere when manufacturing products.

원료질화물 제품이 대기 중에 산소에 급격히 반응하므로 질소분위기에서 제조가 이루어져야 하나 종래는 질화반응과 분쇄공정을 각각 다른 장비로 제조하는 이원화 작업으로 제품이 산소함량이 높고 공정시간도 긴 문제를 가지고 있었다.Since the raw material nitride product reacts rapidly with oxygen in the atmosphere, it must be manufactured in a nitrogen atmosphere, but conventionally, the product has a high oxygen content and a long process time due to the dualization operation of manufacturing the nitriding reaction and the crushing process using different equipment.

본 발명은 상기 문제를 해결하기 위한 것으로, 질화반응과 분쇄공정을 In-line일체화된 제조장치를 제조하여 산소와의 접촉을 최소화하여 산소함량을 줄이고 공정시간을 감소시킬 수 있는 제조방법을 제공하기 위한 것이다.The present invention is to solve the above problems, to provide a manufacturing method that can reduce the oxygen content and reduce the process time by minimizing the contact with oxygen by producing an in-line integrated manufacturing apparatus for the nitriding reaction and grinding process It is for.

상기한 바와 같이 원료질화물 제품의 산소함량을 줄이기 위해 대기 중 노출이 최소화되어야 하며 그러한 이유로 질화반응과 분쇄공정을 In-line일체화가 필요한 부분이다. 질화반응부과 분쇄공정부 사이에 지름 20cm의 연결관을 설치하고 질화반응부 내부에 질소투입구와 분쇄공정부에 질소배출구를 제작하여 상기 두 부의 내부에 질소분위기를 만들어 제조함으로써 대기노출을 최소화 하는 것을 제공한다.As described above, in order to reduce the oxygen content of the raw material nitride product, exposure to the air should be minimized. Therefore, in-line integration of the nitriding reaction and the grinding process is necessary. Minimizing atmospheric exposure by installing a 20 cm diameter connecting tube between the nitriding reaction part and the pulverization process part and by making a nitrogen inlet and a nitrogen outlet in the pulverization process part inside the nitriding reaction part to produce a nitrogen atmosphere inside the two parts. to provide.

분쇄공정부에는 Blade Mixer와 Mesh를 장착하여 분쇄 및 체질을 진행하는 것을 제공한다.The grinding process unit is equipped with blade mixer and mesh to provide grinding and sieving.

질화반응과 분쇄공정을 In-line일체화된 제조장치에서 제조하여 산소와의 접촉을 최소화하여 산소함량을 줄이고 공정시간을 감소시킬 수 있으며, 본 발명의 제조방법을 통하여 산소함량이 낮은 원료질화물을 이용하여 LED 적색형광체를 제조 시 발광강도를 상승시키는 효과가 있다.The nitriding reaction and the pulverization process are manufactured in the in-line integrated manufacturing apparatus to minimize the contact with oxygen, thereby reducing the oxygen content and reducing the process time, and using the raw material nitride having low oxygen content through the manufacturing method of the present invention. Therefore, there is an effect of increasing the emission intensity when manufacturing the LED red phosphor.

도1은 본 발명의 질화반응과 분쇄공정의 In-line화 제조장치를 개략적으로 나타낸 도면이다.
도2는 본 발명의 최종제품인 칼슘질화물(Ca3N2)의 분쇄 후 SEM 사진이다.
도3은 본 발명의 최종제품인 스트론튬질화물(Sr3N2)의 분쇄 후 SEM 사진이다.
도4는 본 발명의 최종제품인 유로퓸질화물(EuN)의 분쇄 후 SEM 사진이다.1 is a view schematically showing an in-line production apparatus of the nitriding reaction and grinding process of the present invention.
Figure 2 is a SEM photograph after the grinding of calcium nitride (Ca 3 N 2 ), the final product of the present invention.
3 is a SEM photograph after grinding of strontium nitride (Sr 3 N 2 ), which is a final product of the present invention.
Figure 4 is a SEM image after the grinding of the europium nitride (EuN) of the final product of the present invention.

이하 첨부된 도면을 참조하여 본 발명을 상세하게 설명한다. 이하에 기재하는 설명은 본 발명의 실시형태의 일례이며 본 발명이 이 실시형태로 한정되는 것은 아니다.DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS The present invention will be described in detail with reference to the accompanying drawings. Description below is an example of embodiment of this invention, and this invention is not limited to this embodiment.

도1은 본 발명의 질화반응과 분쇄공정의 In-line화 제조장치를 개략적으로 나타낸 도면이다.1 is a view schematically showing an in-line production apparatus of the nitriding reaction and grinding process of the present invention.

LED 적색형광체용 원료질화물 In-line화 제조장치에 있어서, 금속원료를 질화하는 질화반응부(1)와 질화된 원료질화물을 분쇄하고 체질하는 분쇄공정부(2)와 질화반응부(1)와 분쇄공정부(2)사이를 연결하는 지름 20cm의 연결관(3)과 질화를 위해 질화반응부(1)에 설치된 질소가스 또는 질소수소혼합가스를 투입하는 질소투입구(4)와 분쇄공정부(2)에 설치되어 투입된 질소가스 또는 질소수소혼합가스를 배출하는 질소배출구(5)로 구성되어 있는 것을 특징으로 한다. 여기서 중요한 역할을 하는 것이 연결관(3)이며 이 연결관(3)의 주된 역할은 질화반응부(1)와 분쇄공정부(2)로 제품이 이동할 때 대기에 노출시키지 않고 질소분위기의 내부이동으로 제품산화를 방지시키는 역할을 하는 것이다.In the in-line production apparatus for the raw material nitride for LED red phosphor, the nitriding reaction part (1) for nitriding metal raw materials, the pulverization process part (2) and the nitriding reaction part (1) for pulverizing and sieving the nitrided raw material nitride A connecting tube 3 having a diameter of 20 cm connecting the grinding process unit 2 and a nitrogen inlet 4 and a grinding process unit for introducing nitrogen gas or nitrogen-hydrogen mixed gas installed in the nitriding reaction unit 1 for nitriding. It is characterized in that it is composed of a nitrogen outlet (5) for discharging the nitrogen gas or nitrogen hydrogen mixed gas introduced and installed in 2). An important role here is the connecting pipe (3) and the main role of the connecting pipe (3) is to move the inside of the nitrogen atmosphere without exposing it to the atmosphere when the product moves to the nitriding reaction part (1) and the grinding process part (2). It is to prevent product oxidation.

질화반응부(1)는 금속원료가 질소 분위기에서 질소 합성되는 질화합성로(1-1)와 설정된 질화반응 조건에 따라 금속원료의 질화 합성을 제어하는 질화합성제어장치(1-2)가 구비되어 있다.The nitriding reaction unit 1 includes a nitriding synthesis furnace 1-1 in which the metal raw material is synthesized in nitrogen in a nitrogen atmosphere and a nitriding synthesis control device 1-2 that controls nitriding synthesis of the metal raw material according to the set nitriding reaction conditions. It is.

분쇄공정부(2)는 질화된 원료질화물을 분쇄하는 분쇄장치(2-1)와 분쇄된 원료질화물을 체질하는 Mesh(2-2)를 포함하고 있으며 제품의 출입을 위한 제품출입구(2-3)가 구비되어있다.The grinding process unit 2 includes a crushing apparatus 2-1 for pulverizing the nitrided raw material nitride and a mesh 2-2 for sieving the pulverized raw nitride, and the product entrance and exit for the product entry and exit (2-3). ) Is equipped.

또한 분쇄공정부(2)는 분쇄공정부(2)에서 질화반응부(1)로 또는 질화반응부(1)에서 분쇄공정부(2)로 상기 연결관(3)의 내부를 통해서 금속 원료물질 및 질화된 원료질화물 제품을 이동시키는 이동장치(2-4)가 구비되어 있으며, 이동장치(2-4)는 제품도가니를 놓을 수 있는 홀더에 5mm두께의 이동연결관(2-5)이 부착되어 있으며 이동연결관(2-5)의 10cm는 분쇄공정부(2) 외부에 돌출되어 있는 형태로 구성되어 있다. 이 돌출되어 있는 이동연결관(2-5)을 잡고 이동시켜 원료물질 및 질화물제품을 이동시킬 수 있다.In addition, the grinding process unit 2 is a metal raw material through the interior of the connecting pipe 3 from the grinding process unit 2 to the nitriding reaction unit 1 or from the nitriding reaction unit 1 to the grinding process unit 2. And a moving device (2-4) for moving the nitrided raw material nitride product, and the moving device (2-4) has a 5 mm-thick moving connecting pipe (2-5) attached to a holder for placing a product crucible. 10cm of the mobile connection pipe (2-5) is configured to protrude to the outside of the grinding process unit (2). By holding and moving the protruding movable connecting pipe 2-5, the raw material and the nitride product can be moved.

상기 질화반응부(1)와 분쇄공정부(2)의 내부에 질소분위기를 만들어 제조함으로써 대기노출을 최소화하는 것이다.By minimizing the atmospheric exposure by making a nitrogen atmosphere in the nitriding reaction unit (1) and the grinding process unit (2).

또한 본 발명은 LED 적색형광체용 원료질화물 In-line화 제조방법에 있어서,In addition, the present invention is a method for producing a raw material nitride in-line for the LED red phosphor,

(a) 질화반응과 분쇄공정을 In-line일체화하여 질소분위기의 질화반응부(1) 내부에서 금속원료를 질화하여 산소오염을 최소화하는 질화반응 단계와,(a) a nitriding reaction step of minimizing oxygen contamination by nitriding metal raw materials in the nitriding reaction part (1) of the nitrogen atmosphere by in-line integrating the nitriding reaction and the grinding process;

(b) 질화된 질화반응물을 질소분위기의 분쇄공정부(2)의 내부에 있는 분쇄장치(2-1)로 분쇄하는 단계와,(b) pulverizing the nitriding nitride with a pulverizing device 2-1 in the pulverizing unit 2 of the nitrogen atmosphere;

(c) 분쇄된 질화반응물을 질소분위기의 분쇄공정부(2)의 내부에 있는 Mesh(2-2)로 체질하는 단계로 구성된 것을 특징으로 한다.(c) sieving the pulverized nitride reactant with a mesh (2-2) in the interior of the pulverization process unit 2 of the nitrogen atmosphere.

더욱 상세하게는 원료질화물 제품에 대한 제조방법은 단계(a)에서 제조원료인 금속원료(순도 99.99%이상)를 분쇄공정부(2)의 제품출입구(2-3)에 투입 후 이동장치(2-4)에 의해 연결관(3) 내부를 통해 질화반응부(1)의 질화합성로(1-1)로 이동시킨다. 금속원료가 질화공정부(1)의 질화합성로(1-1)로 이동된 후 질화합성제어장치(1-2)의 제어를 통해 설정된 질화반응 조건으로 질화반응을 한다. 질화반응은 700~900의 온도로 반응하며 승온시간은 5/min이며 이때 질화반응부(1) 내부로 질소투입구(4)를 통해 질소가스를 0.5L/min의 량으로 투입하며 2~8시간 동안 반응을 실시한다. 단계(b)에서 반응 종료 후 질화된 질화반응물이 이동장치(2-4)에 의해 연결관(3) 내부를 통해 분쇄공정부(2)로 이동되어 분쇄장치(2-1)인 Blade Mixer를 이용하여 분쇄를 실시한 후, 단계(c)에서 Mesh(2-2)를 사용하여 체질을 한다. 체질이 완료된 후 투입된 질소를 질소배출구(5)를 통해 질소를 배출시킨 후 완료된 제품을 제품출입구(2-3)를 통해 배출한다.More specifically, the manufacturing method for the raw material nitride product is a metal raw material (purity 99.99% or more) of the raw material in the step (a) is introduced into the product entrance (2-3) of the grinding process unit 2 and then the moving device (2). -4) is moved to the nitriding synthesis furnace (1-1) of the nitriding reaction part (1) through the inside of the connecting pipe (3). After the metal raw material is moved to the nitriding synthesis furnace 1-1 of the nitriding process unit 1, the nitriding reaction is performed under the nitriding reaction conditions set through the control of the nitriding synthesis control device 1-2. The nitriding reaction is carried out at a temperature of 700 to 900 and the temperature increase time is 5 / min. At this time, nitrogen gas is introduced into the nitriding reaction unit 1 through a nitrogen inlet 4 at a rate of 0.5 L / min for 2 to 8 hours. During the reaction. After the reaction is completed in step (b), the nitrided nitride reactant is moved to the grinding process unit 2 through the connection pipe 3 by the moving device 2-4 to move the blade mixer, the grinding device 2-1. After the pulverization by using, in the step (c) to sieve using the Mesh (2-2). After the sieving is completed, the injected nitrogen is discharged through the nitrogen discharge port 5, and then the finished product is discharged through the product entrance (2-3).

본 발명의 LED 적색형광체용 원료질화물은 99.9% 이상의 고순도 금속원료를 질소가스 또는 질소수소혼합가스를 사용하여 상압에서 질화 반응시켜 제품을 제조하는 방법으로 유사한 제조방법으로 초음파 질화법, 암모니아가스 질화법, 염욕 질화법 등이 있다.The raw material nitride for LED red phosphor of the present invention is a method of producing a product by nitriding a high purity metal raw material of 99.9% or more at normal pressure using nitrogen gas or nitrogen hydrogen mixed gas. , Salt bath nitriding, etc.

본 발명에서는 Ca, Sr 및 Eu 금속을 각각 별도로 잘화반응을 시킬 수도 있고, 이들 금속중 2 또는 3종의 금속을 함께 질화반응을 시킬 수도 있다. 이렇게 하면, 반응시간의 단축이 가능하며, 더욱 효율적으로 고순도의 금속질화물을 제조할 수 있다.In the present invention, Ca, Sr, and Eu metals may be reacted with each other separately, or two or three metals among these metals may be nitrided together. In this way, reaction time can be shortened and metal nitride of high purity can be manufactured more efficiently.

원료질화물의 질화반응을 높이기 위하여 700에서 900사이의 온도에서 질화반응을 진행하며 질화물제품에 따라 설정 온도조건이 다르다. 일반적으로 700미만에서 반응 시 질화반응이 제대로 이루어 지지 않으며 900 초과에서 반응 시 제품이 녹아내릴 수 있다. 질화반응 시간은 2시간에서 8시간 사이에서 반응하며 이 역시 제품의 종류에 따라 설정 시간이 다르며 2시간 미만 반응시 질화반응이 제대로 이루어 지지 않아 제품의 질소함량이 낮을 수 있고 8시간 초과 시 제품의 산소농도가 증가한다.In order to increase the nitriding reaction of the raw material nitride, the nitriding reaction is carried out at a temperature between 700 and 900, and the set temperature conditions are different depending on the nitride products. In general, when the reaction is less than 700, the nitriding reaction is not performed properly, and if it is more than 900, the product may melt. The nitriding reaction time is between 2 hours and 8 hours.The setting time also varies depending on the type of product. If the reaction time is less than 2 hours, the nitrification reaction is not properly performed. Therefore, the nitrogen content of the product may be low. Oxygen concentration increases.

질화반응 시 본 발명의 핵심인 In-line화 된 제조장치에서 제조하며 유사한 제조설비방식으로는 진공식(Vacuum), 배치식(Batch), 메쉬벨트식(Mesh belt) 등이 있다.In the nitriding reaction, the core of the present invention is manufactured in an in-lined manufacturing apparatus, and similar manufacturing equipment includes vacuum, batch, mesh belt, and the like.

원료질화물 분쇄는 질소분위기 분쇄공정부 내부에 있는 Blade Mixer(내부용량2L)를 이용하여 분쇄하며 회당 100g, 분쇄시간은 5±1 min, blade속도는 22,000±1000 rpm으로 분쇄된다.The raw material nitride is pulverized using Blade Mixer (internal capacity 2L) inside the nitrogen atmosphere crushing process unit, and it is pulverized at 100g per hour, grinding time is 5 ± 1 min, and blade speed is 22,000 ± 1000 rpm.

원료질화물은 최대크기 53이하에서 관리해야 하며 질소분위기 분쇄공정부 내부에 있는 Mesh(눈금크기 53)를 사용하여 체질을 진행하여 최종제품을 제조한다.The raw material nitride should be managed under the maximum size of 53 or less, and the final product is manufactured by sieving using the mesh (scale size 53) inside the nitrogen atmosphere crushing process unit.

상기의 모든 과정이 질소분위기에서 진행되어야 하며 산소유입을 최소화하기 위하여 In-line화 제조방법이 진행된다.All of the above process must be carried out in a nitrogen atmosphere and the in-line production process is performed to minimize the oxygen inflow.

원료질화물 내 산소유입이 최소화될 경우 원자재 순도가 향상되어 LED적색형광체 제조 시 형광체 순도도 함께 향상되어 발광강도특성이 상승하는 효과를 가질 수 있다.When oxygen inflow is minimized in raw material nitride, the purity of raw materials is improved, and the purity of phosphors is also improved when LED red phosphors are manufactured.

제조원료인 Ca Metal(순도 99.99%이상)을 분쇄공정부(2)의 제품출입구(2-3)에 투입 후 질화반응부(1)의 질화합성로(1-1)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시겼다. Ca Metal이 질화공정부(1)의 질화합성로(1-1)로 이동된 후 질화합성제어장치(1-2)의 제어를 통해 설정된 질화반응 조건으로 질화반응 시켰다. 이때 질화반응 조건은 700의 온도, 승온시간은 5/min으로 반응시켰으며 이때 질화반응부(1) 내부로 질소투입구(4)를 통해 순도 99.99%의 질소가스를 0.5L/min의 량으로 투입하며 2시간 동안 반응을 실시했다. 반응이 종료된 후 질화된 질화반응물을 이동장치(2-4)에 의해 연결관(3) 내부를 통해 분쇄공정부(2)로 이동시켜 분쇄장치(2-1)인 Blade Mixer를 이용하여 분쇄를 실시한 후, 53의 Mesh(2-2)를 사용하여 체질을 하여 원료질화물이 16.88% 이상 질화반응된 칼슘질화물(Ca3N2)을 제조했다. Ca Metal (purity 99.99% or more), which is a raw material, is introduced into the product entrance (2-3) of the grinding process unit (2), and then moved to the nitriding synthesis furnace (1-1) of the nitriding reaction unit (1). 4) through the inside of the connecting pipe (3). Ca metal was moved to the nitriding synthesis furnace (1-1) of the nitriding process (1) and nitrified under the nitriding reaction conditions set through the control of the nitriding synthesis controller (1-2). In this case, the nitriding reaction was performed at a temperature of 700 and a temperature increase time was 5 / min. At this time, nitrogen gas having a purity of 99.99% was introduced into the nitriding reaction unit 1 through a nitrogen inlet 4 at a rate of 0.5 L / min. The reaction was carried out for 2 hours. After the reaction is completed, the nitrided nitride is moved to the pulverization process unit 2 through the inside of the connecting pipe 3 by the moving device 2-4, and pulverized using the blade mixer, which is the pulverizing device 2-1. After the sieving, sieving was carried out using 53 Mesh (2-2) to prepare calcium nitride (Ca 3 N 2 ) having a nitride of at least 16.88%.

최종제품인 칼슘질화물(Ca3N2)의 분쇄 후의 OHN가스분석기를 이용하여 측정된 질소 및 산소함량을 종래의 원료질화물과 비교한 결과를 표 1에 나타내었으며, SEM에 의한 사진을 도 2에 나타냈다. 종래의 방법에 의해 제조된 원료질화물(Ca3N2)과 본 발명의 제조방법에 따른 산소함량이 낮은 원료질화물(Ca3N2)을 이용하여 LED적색형광체를 제조하여 형광체 발광강도측정이 가능한 PL분석장비를 이용하여 분석한 DATA를 가지고 비교한 결과를 표 2에 나타냈다.Table 1 shows the results of comparing the nitrogen and oxygen content measured using the OHN gas analyzer after the pulverization of the final product, calcium nitride (Ca 3 N 2 ), with the conventional raw material nitride, and the SEM photograph is shown in FIG. 2. . Using a raw nitride (Ca 3 N 2) and a lower raw material nitride oxygen content (Ca 3 N 2) according to the production method of the present invention prepared by a conventional method to prepare a LED red phosphor capable of fluorescent emission intensity measured Table 2 shows the result of comparing the data analyzed using the PL analysis equipment.

종래 원료질화물
(Ca3N2)가스함량분석(단위:wt%)Conventional raw material nitride
(Ca 3 N 2 ) Gas content analysis (unit: wt%) 본 발명 원료질화물
(Ca3N2)가스함량분석(단위:wt%)Raw material nitride of the present invention
(Ca 3 N 2 ) Gas content analysis (unit: wt%) 질소nitrogen 산소Oxygen 질소nitrogen 산소Oxygen 1회1 time 15.8915.89 0.610.61 17.1017.10 0.310.31 2회Episode 2 15.5615.56 0.640.64 16.9916.99 0.330.33 3회3rd time 16.5016.50 0.550.55 17.5217.52 0.290.29 4회4 times 15.2615.26 0.630.63 16.9216.92 0.340.34 5회5 times 16.5216.52 0.540.54 17.3317.33 0.310.31 6회6 times 15.6815.68 0.640.64 17.3017.30 0.310.31 7회7 times 15.7915.79 0.630.63 16.9316.93 0.340.34 8회8 times 15.5715.57 0.660.66 17.3517.35 0.300.30 9회9 times 16.4816.48 0.520.52 17.5017.50 0.280.28 10회10 times 15.9515.95 0.560.56 16.8816.88 0.350.35 평균Average 15.92 15.92 0.60 0.60 17.12 17.12 0.32 0.32

종래 원료질화물
(Ca3N2)제품적용(단위:cps)Conventional raw material nitride
(Ca 3 N 2 ) Product Application (Unit: cps) 본 발명 원료질화물
(Ca3N2)제품적용(단위:cps)Raw material nitride of the present invention
(Ca 3 N 2 ) Product Application (Unit: cps) 1회1 time 454454 494494 2회Episode 2 443443 493493 3회3rd time 461461 499499 4회4 times 438438 489489 5회5 times 458458 497497 6회6 times 446446 498498 7회7 times 451451 495495 8회8 times 436436 498498 9회9 times 458458 499499 10회10 times 447447 489489 평균Average 449 449 495 495

상기 표 2에서와 같이 본 발명의 제조장치 및 방법을 통하여 산소함량이 낮은 원료질화물을 이용하여 LED적색형광체를 제조 시 발광강도를 10% 상승시키는 효과를 보였다.As shown in Table 2, through the manufacturing apparatus and method of the present invention, the emission intensity was increased by 10% when the LED red phosphor was manufactured using a raw material nitride having a low oxygen content.

제조원료인 Sr Metal(순도 99.99%이상)을 분쇄공정부(2)의 제품출입구(2-3)에 투입 후 질화반응부(1)의 질화합성로(1-1)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시겼다. Sr Metal이 질화공정부(1)의 질화합성로(1-1)로 이동된 후 질화합성제어장치(1-2)의 제어를 통해 설정된 질화반응 조건으로 질화반응 시켰다. 이때 질화반응 조건은 900의 온도, 승온시간은 5/min으로 반응시켰으며 이때 질화반응부(1) 내부로 질소투입구(4)를 통해 순도 99.99%의 질소와 순도 99.99%의 수소를 함량비 질소:수소 = 95:5로 0.5L/min의 량으로 투입하며 8시간 동안 반응을 실시했다. 반응이 종료된 후 질화된 질화반응물을 분쇄공정부(2)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시켜 분쇄장치(2-1)인 Blade Mixer를 이용하여 분쇄를 실시한 후, 53의 Mesh(2-2)를 사용하여 체질을 하여 7.90% 이상 질화반응된 스트론튬 질화물(Sr3N2)을 제조했다.Sr Metal (purity 99.99% or more), which is a raw material, is introduced into the product entrance (2-3) of the grinding process unit (2), and then moved to the nitriding synthesis furnace (1-1) of the nitriding reaction unit (1). 4) through the inside of the connecting pipe (3). Sr Metal was moved to the nitriding synthesis furnace 1-1 of the nitriding process unit 1 and subjected to nitriding reaction under the nitriding reaction conditions set through the control of the nitriding synthesis control device 1-2. At this time, the nitriding reaction was carried out at a temperature of 900, and the temperature increase time was 5 / min. At this time, the nitrogen inlet (1) contained nitrogen having a purity of 99.99% and hydrogen having a purity of 99.99% through a nitrogen inlet (4). The reaction was carried out for 8 hours with hydrogen = 95: 5 at a rate of 0.5 L / min. After the reaction is completed, the nitriding nitride is moved to the grinding process unit 2 by the moving device 2-4 through the inside of the connecting pipe 3 and ground using the blade mixer, which is the grinding device 2-1. After the sieving, sieving was carried out using 53 Mesh (2-2) to prepare strontium nitride (Sr 3 N 2 ) which was at least 7.90% nitrided.

최종제품인 스트론튬질화물(Sr3N2)의 분쇄 후의 OHN가스분석기를 이용하여 측정된 질소 및 산소함량을 종래의 원료질화물과 비교한 결과를 표 3에 나타내었으며, SEM에 의한 사진을 도 3에 나타냈다. 종래의 방법에 의해 제조된 원료질화물(Sr3N2)과 본 발명의 제조방법에 따른 산소함량이 낮은 원료질화물(Sr3N2)을 이용하여 LED적색형광체를 제조하여 형광체 발광강도측정이 가능한 PL분석장비를 이용하여 분석한 DATA를 가지고 비교한 결과를 표 4에 나타냈다.Table 3 shows the results of comparing the nitrogen and oxygen content measured using the OHN gas analyzer after crushing the final product of strontium nitride (Sr 3 N 2 ) with the conventional raw material nitride, and the SEM photograph is shown in FIG. 3. . Using a raw nitride (Sr 3 N 2) and a lower raw material nitride oxygen content (Sr 3 N 2) according to the production method of the present invention prepared by a conventional method to prepare a LED red phosphor capable of fluorescent emission intensity measured Table 4 shows the result of comparing the data analyzed using the PL analysis equipment.

종래 원료질화물
(Sr3N2)가스함량분석(단위:wt%)Conventional raw material nitride
(Sr 3 N 2 ) Gas content analysis (unit: wt%) 본 발명 원료질화물
(Sr3N2)가스함량분석(단위:wt%)Raw material nitride of the present invention
(Sr 3 N 2 ) Gas content analysis (unit: wt%) 질소nitrogen 산소Oxygen 질소nitrogen 산소Oxygen 1회1 time 6.926.92 0.590.59 8.128.12 0.280.28 2회Episode 2 7.117.11 0.520.52 8.158.15 0.260.26 3회3rd time 7.187.18 0.500.50 7.997.99 0.300.30 4회4 times 6.946.94 0.570.57 8.058.05 0.290.29 5회5 times 6.916.91 0.600.60 8.088.08 0.300.30 6회6 times 7.097.09 0.520.52 7.917.91 0.350.35 7회7 times 6.896.89 0.620.62 7.947.94 0.340.34 8회8 times 7.137.13 0.510.51 8.008.00 0.300.30 9회9 times 6.956.95 0.580.58 7.967.96 0.330.33 10회10 times 7.107.10 0.520.52 8.118.11 0.280.28 평균Average 7.02 7.02 0.55 0.55 8.03 8.03 0.30 0.30

종래 원료질화물
(Sr3N2)제품적용(단위:cps)Conventional raw material nitride
(Sr 3 N 2 ) Product Application (Unit: cps) 본 발명 원료질화물
(Sr3N2)제품적용(단위:cps)Raw material nitride of the present invention
(Sr 3 N 2 ) Product Application (Unit: cps) 1회1 time 439439 497497 2회Episode 2 446446 499499 3회3rd time 451451 491491 4회4 times 441441 496496 5회5 times 439439 497497 6회6 times 444444 488488 7회7 times 436436 494494 8회8 times 447447 491491 9회9 times 441441 489489 10회10 times 446446 498498 평균Average 443 443 494 494

상기 표 4에서와 같이 본 발명의 제조장치 및 방법을 통하여 산소함량이 낮은 원료질화물을 이용하여 LED적색형광체를 제조 시 발광강도를 12% 상승시키는 효과를 보였다.As shown in Table 4, through the production apparatus and method of the present invention, the emission intensity was increased by 12% when the LED red phosphor was manufactured using a raw material nitride having a low oxygen content.

제조원료인 Eu Metal(순도 99.99%이상)을 분쇄공정부(2)의 제품출입구(2-3)에 투입 후 질화반응부(1)의 질화합성로(1-1)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시겼다. Eu Metal이 질화공정부(1)의 질화합성로(1-1)로 이동된 후 질화합성제어장치(1-2)의 제어를 통해 설정된 질화반응 조건으로 질화반응 시켰다. 이때 질화반응 조건은 900의 온도, 승온시간은 5/min으로 반응시켰으며 이때 질화반응부(1) 내부로 질소투입구(4)를 통해 순도 99.99%의 질소와 순도 99.99%의 수소를 함량비 질소:수소 = 90:10로 0.5L/min의 량으로 투입하며 8시간 동안 반응을 실시했다. 반응이 종료된 후 질화된 질화반응물을 분쇄공정부(2)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시켜 분쇄장치(2-1)인 Blade Mixer를 이용하여 분쇄를 실시한 후, 53의 Mesh(2-2)를 사용하여 체질을 하여 8.97% 이상 질화반응된 유로퓸질화물(EuN)을 제조했다.Eu Metal (purity 99.99% or more), which is a raw material, is introduced into the product inlet (2-3) of the grinding process unit (2), and then moved to the nitriding synthesis furnace (1-1) of the nitriding reaction unit (1). 4) through the inside of the connecting pipe (3). Eu Metal was moved to the nitriding synthesis furnace (1-1) of the nitriding process (1) and subjected to nitriding reaction under the nitriding reaction conditions set through the control of the nitriding synthesis control device (1-2). At this time, the nitriding reaction was carried out at a temperature of 900, and the temperature increase time was 5 / min. At this time, the nitrogen inlet (1) contained nitrogen having a purity of 99.99% and hydrogen having a purity of 99.99% through a nitrogen inlet (4). : Hydrogen = 90:10 The reaction was carried out for 8 hours with an amount of 0.5 L / min. After the reaction is completed, the nitriding nitride is moved to the grinding process unit 2 by the moving device 2-4 through the inside of the connecting pipe 3 and ground using the blade mixer, which is the grinding device 2-1. After performing the sieving using 53 (2-2), 53 was nitrated over 8.97% to produce europium nitride (EuN).

최종제품인 유로퓸질화물(EuN)의 분쇄 후의 OHN가스분석기를 이용하여 측정된 질소 및 산소함량을 종래의 원료질화물과 비교한 결과를 표 5에 나타내었으며, SEM에 의한 사진을 도 4에 나타냈다. 종래의 방법에 의해 제조된 원료질화물(EuN)과 본 발명의 제조방법에 따른 산소함량이 낮은 원료질화물(EuN)을 이용하여 LED적색형광체를 제조하여 형광체 발광강도측정이 가능한 PL분석장비를 이용하여 분석한 DATA를 가지고 비교한 결과를 표 6에 나타냈다.Table 5 shows the results of comparing the nitrogen and oxygen content measured using the OHN gas analyzer after the pulverization of the final product Europium nitride (EuN) with the conventional raw material nitride, and the photograph by SEM is shown in FIG. Using a PL analysis device capable of measuring phosphor emission intensity by manufacturing LED red phosphor using raw material nitride (EuN) prepared by a conventional method and raw material nitride (EuN) having low oxygen content according to the manufacturing method of the present invention Table 6 shows the results of the comparison with the analyzed data.

종래 원료질화물
(EuN)가스함량분석(단위:wt%)Conventional raw material nitride
(EuN) Gas content analysis (unit: wt%) 본 발명 원료질화물
(EuN)가스함량분석(단위:wt%)Raw material nitride of the present invention
(EuN) Gas content analysis (unit: wt%) 질소nitrogen 산소Oxygen 질소nitrogen 산소Oxygen 1회1 time 8.688.68 0.480.48 8.998.99 0.330.33 2회Episode 2 8.608.60 0.580.58 9.069.06 0.300.30 3회3rd time 8.548.54 0.660.66 9.189.18 0.240.24 4회4 times 8.658.65 0.510.51 9.099.09 0.280.28 5회5 times 8.678.67 0.500.50 9.109.10 0.270.27 6회6 times 8.628.62 0.520.52 9.059.05 0.300.30 7회7 times 8.628.62 0.530.53 9.039.03 0.310.31 8회8 times 8.608.60 0.540.54 9.139.13 0.260.26 9회9 times 8.698.69 0.470.47 8.978.97 0.340.34 10회10 times 8.568.56 0.640.64 9.099.09 0.270.27 평균Average 8.62 8.62 0.54 0.54 9.07 9.07 0.29 0.29

종래 원료질화물
(EuN)제품적용(단위:cps)Conventional raw material nitride
(EuN) Product Application (Unit: cps) 본 발명 원료질화물
(EuN)제품적용(단위:cps)Raw material nitride of the present invention
(EuN) Product Application (Unit: cps) 1회1 time 459459 484484 2회Episode 2 451451 488488 3회3rd time 447447 497497 4회4 times 456456 490490 5회5 times 459459 491 491 6회6 times 454454 488488 7회7 times 456456 486486 8회8 times 450450 494494 9회9 times 459459 482482 10회10 times 449 449 490490 평균 Average 454 454 489 489

상기 표 6에서와 같이 본 발명의 제조장치 및 방법을 통하여 산소함량이 낮은 원료질화물을 이용하여 LED적색형광체를 제조 시 발광강도를 8% 상승시키는 효과를 보였다.As shown in Table 6, through the manufacturing apparatus and method of the present invention, the emission intensity was increased by 8% when the LED red phosphor was manufactured using a raw material nitride having a low oxygen content.

제조원료인 Ca Metal(순도 99.99%이상), Sr Metal(순도 99.99%이상), Eu Metal(순도 99.99%이상)을 각각 Ca-0.2mol, Sr-0.76mol, Eu-0.04mol 칭량한 후 분쇄공정부(2)의 제품출입구(2-3)에 투입 후 질화반응부(1)의 질화합성로(1-1)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시겼다. 이 금속이 질화공정부(1)의 질화합성로(1-1)로 이동된 후 질화합성제어장치(1-2)의 제어를 통해 설정된 질화반응 조건으로 질화반응 시켰다. 이때 질화반응 조건은 900의 온도, 승온시간은 5/min으로 반응시켰으며 이때 질화반응부(1) 내부로 질소투입구(4)를 통해 순도 99.99%의 질소와 순도 99.99%의 수소를 함량비 질소:수소 = 90:10로 0.5L/min의 량으로 투입하며 8시간 동안 반응을 실시했다. 반응이 종료된 후 질화된 질화반응물을 분쇄공정부(2)로 이동장치(2-4)에 의해 연결관(3) 내부를 통해 이동시켜 분쇄장치(2-1)인 Blade Mixer를 이용하여 분쇄를 실시한 후, 53의 Mesh(2-2)를 사용하여 체질을 하여 9.65% 이상 질화반응된 질화물을 제조했다.Ca-0.2mol, Sr-0.76mol, Eu-0.04mol weighing Ca Metal (purity 99.99%), Sr Metal (purity 99.99%) and Eu Metal (purity 99.99%) respectively After inputting into the product entrance (2-3) of the government (2), it was moved through the connecting pipe (3) by the moving device (2-4) to the nitriding synthesis furnace (1-1) of the nitriding reaction part (1). . The metal was moved to the nitriding synthesis furnace 1-1 of the nitriding process unit 1 and subjected to nitriding reaction under the nitriding reaction conditions set through the control of the nitriding synthesis control device 1-2. At this time, the nitriding reaction was carried out at a temperature of 900, and the temperature increase time was 5 / min. At this time, the nitrogen inlet (1) contained nitrogen having a purity of 99.99% and hydrogen having a purity of 99.99% through a nitrogen inlet (4). : Hydrogen = 90:10 The reaction was carried out for 8 hours with an amount of 0.5 L / min. After the reaction is completed, the nitriding nitride is moved to the grinding process unit 2 by the moving device 2-4 through the inside of the connecting pipe 3 and ground using the blade mixer, which is the grinding device 2-1. After performing the sieving using the Mesh (2-2) of 53 to prepare a nitrided nitride of 9.65% or more.

최종제품인 질화물의 분쇄 후의 OHN가스분석기를 이용하여 측정된 질소 및 산소함량을 종래의 원료질화물과 비교한 결과를 표 7에 나타내었다. 종래의 방법에 의해 제조된 각각의 원료질화물과 본 발명의 제조방법에 따른 산소함량이 낮은 원료질화물을 이용하여 LED적색형광체를 제조하여 형광체 발광강도측정이 가능한 PL분석장비를 이용하여 분석한 DATA를 가지고 비교한 결과를 표 8에 나타냈다.Table 7 shows the results of comparing the nitrogen and oxygen content measured using the OHN gas analyzer after crushing the final product nitride with the conventional raw material nitride. Using the PL analysis equipment capable of measuring the phosphor emission intensity by producing LED red phosphor using each of the raw material nitrides prepared by the conventional method and the raw material nitrides having low oxygen content according to the production method of the present invention, the analyzed data were analyzed. Table 8 shows the result of the comparison.

종래 원료질화물
가스함량분석(단위:wt%)Conventional raw material nitride
Gas content analysis (unit: wt%) 본 발명 원료질화물
가스함량분석(단위:wt%)Raw material nitride of the present invention
Gas content analysis (unit: wt%) 질소nitrogen 산소Oxygen 질소nitrogen 산소Oxygen 1회1 time 9.469.46 0.490.49 9.699.69 0.330.33 2회Episode 2 9.359.35 0.520.52 9.759.75 0.310.31 3회3rd time 9.559.55 0.460.46 9.669.66 0.340.34 4회4 times 9.449.44 0.480.48 9.819.81 0.280.28 5회5 times 9.409.40 0.520.52 9.759.75 0.30.3 6회6 times 9.369.36 0.550.55 9.719.71 0.320.32 7회7 times 9.599.59 0.450.45 9.829.82 0.280.28 8회8 times 9.569.56 0.450.45 9.689.68 0.260.26 9회9 times 9.429.42 0.470.47 9.779.77 0.340.34 10회10 times 9.419.41 0.490.49 9.739.73 0.330.33 평균Average 9.45 9.45 0.49 0.49 9.74 9.74 0.310.31

종래 원료질화물
제품적용(단위:cps)Conventional raw material nitride
Product Application (Unit: cps) 본 발명 원료질화물
제품적용(단위:cps)Raw material nitride of the present invention
Product Application (Unit: cps) 1회1 time 448448 481481 2회Episode 2 440440 484484 3회3rd time 458458 480480 4회4 times 450450 487487 5회5 times 442442 483483 6회6 times 440440 482482 7회7 times 450450 489489 8회8 times 447447 481481 9회9 times 443443 484484 10회10 times 443443 482482 평균Average 446 446 483 483

상기 표 8에서와 같이 본 발명의 제조장치 및 방법을 통하여 산소함량이 낮은 원료질화물을 이용하여 LED적색형광체를 제조 시 발광강도를 11% 상승시키는 효과를 보였다.
As shown in Table 8, when the LED red phosphor was manufactured using a raw material nitride having a low oxygen content, the emission intensity was increased by 11% through the manufacturing apparatus and method of the present invention.

1. 질화반응부 2, 분쇄공정부
1-1. 질화합성로 2-1. 분쇄장치
1-2. 질화합성제어장치 2-2. Mesh
3. 연결관 2-3. 제품출입구
4. 질소투입구 2-4. 이동장치
5. 질소배출구 2-5. 이동연결관1. Nitriding reaction part 2, grinding process part
1-1. Nitriding furnace 2-1. Crusher
1-2. Nitride Compounding Control Device 2-2. Mesh
3. Connector 2-3. Product entrance
4. Nitrogen Inlet 2-4. Mobile device
5. Nitrogen outlet 2-5. Transfer connector

Claims (12)

(a) 질화반응과 분쇄공정을 In-line일체화하여 질소분위기의 질화반응부 내부에서 금속원료를 질화하여 산소오염을 최소화하는 질화반응 단계와,
(b) 질화된 질화반응물을 질소분위기의 분쇄공정부의 내부에 있는 분쇄장치로 분쇄하는 단계와,
(c) 분쇄된 질화반응물을 질소분위기의 분쇄공정부의 내부에 있는 Mesh로 체질하는 단계로 구성된 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.(a) nitriding reaction step of minimizing oxygen contamination by nitriding metal raw materials in nitriding reaction part of nitrogen atmosphere by in-line integration of nitriding reaction and grinding process;
(b) pulverizing the nitrided nitride with a pulverizer in the pulverization process section of the nitrogen atmosphere;
(C) a method of manufacturing a raw material nitride in-line for the LED red phosphor, characterized in that the pulverized nitrate reacted to a mesh inside the pulverization process of the nitrogen atmosphere. 제 1항에 있어서,
질화시킬 금속 Ca, Sr 및 Eu를 각각 단독으로 질화시키거나 또는 2 내지 3종의 금속을 함께 질화시키는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
A process for producing a raw material nitride in-line for an LED red phosphor, characterized in that the metals to be nitrided are each nitrided with Ca, Sr, and Eu alone or with two or three metals together. 제 1항에 있어서,
질화반응 된 Ca3N2, Sr3N2, EuN 내 산소함량이 0.35wt% 이하를 갖는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
A method for producing a raw material nitride in-line for an LED red phosphor, characterized in that the oxygen content of nitrified Ca 3 N 2 , Sr 3 N 2 , EuN is 0.35 wt% or less. 제 1항에 있어서,
원료질화물의 질화반응을 높이기 위하여 700에서 900사이의 온도에서, 시간은 2시간에서 8시간 사이에서 질화반응하는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
In order to increase the nitriding reaction of the raw material nitride at the temperature of 700 to 900, the time is nitriding reaction between 2 hours and 8 hours, characterized in that the raw material nitride in-line production method for red phosphor LED. 제 1항에 있어서,
단계(a)에서 원료질화물이 16.88% 이상 질화반응된 칼슘질화물(Ca3N2)인 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
Raw material nitride in the step (a) 16.88% or more nitrified calcium nitride (Ca 3 N 2 ) characterized in that the raw material nitride in-line production method for red phosphor LED. 제 1항에 있어서,
단계(a)에서 원료질화물이 7.90% 이상 질화반응된 스트론튬질화물(Sr3N2)인 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
Raw material nitride in step (a) is 7.90% or more nitriding reaction of strontium nitride (Sr 3 N 2 ) characterized in that the raw material nitride in-line production method for red phosphor LED. 제 1항에 있어서,
단계(a)에서 원료질화물이 8.97% 이상 질화반응된 유로퓸질화물(EuN)인 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
Raw material nitride in step (a) is 8.97% or more nitrified europium nitride (EuN) characterized in that the raw material nitride in-line production method for red phosphor LED. 제 1항에 있어서,
단계(b)에서 blade mixer를 이용하여 기계적으로 원료질화물을 분쇄하는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
The raw material nitride in-line manufacturing method for the LED red phosphor, characterized in that the raw material nitride is mechanically ground using a blade mixer in step (b). 제 1항에 있어서,
단계(c)에서 Mesh의 눈금크기는 53인 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method of claim 1,
In step (c) the grid size of the raw material nitride in-line production method for the LED red phosphor, characterized in that 53. 제 6항에 있어서,
원료질화물의 분쇄는 회당 100g, 분쇄시간은 5±1 min, blade속도는 22,000±1000 rpm으로 하는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조방법.The method according to claim 6,
Raw material nitride is pulverized 100g per time, grinding time is 5 ± 1 min, blade speed is 22,000 ± 1000 rpm, characterized in that the raw material nitride in-line production method for red phosphor LED. LED 적색형광체용 원료질화물 In-line화 제조장치에 있어서,
금속원료를 질화하는 질화반응부와, 질화된 원료질화물을 분쇄하고 체질하는 분쇄공정부와, 상기 질화반응부와 상기 분쇄공정부 사이를 연결하는 연결관과, 질화를 위해 상기 질화반응부에 설치된 질소가스 또는 질소수소혼합가스를 투입하는 질소투입구와, 상기 분쇄공정부에 설치되어 투입된 질소가스 또는 질소수소혼합가스를 배출하는 질소배출구로 구성되어 있으며,
상기 질화반응부는 금속원료가 질소 분위기에서 질소 합성되는 질화합성로와 설정된 질화반응 조건에 따라 금속원료의 질화 합성을 제어하는 질화합성제어장치를 포함하며,
상기 분쇄공정부는 질화된 원료질화물을 분쇄하는 분쇄장치와 분쇄된 원료질화물을 체질하는 Mesh를 포함하고 있으며 제품의 출입을 위한 제품출입구가 포함되어 있으며, 상기 분쇄공정부에서 상기 질화반응부로 또는 질화반응부에서 상기 분쇄공정부로 상기 연결관의 내부를 통해서 금속원료 또는 질화된 원료질화물을 이동시키는 이동장치가 구비되어 있는 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조장치.In the raw material nitride in-line manufacturing apparatus for LED red phosphor,
A nitriding reaction unit for nitriding metal raw materials, a pulverizing process unit for pulverizing and sieving nitrided raw material nitride, a connecting pipe connecting the nitriding reaction unit and the crushing process unit, and the nitriding reaction unit for nitriding It is composed of a nitrogen inlet for injecting nitrogen gas or nitrogen-hydrogen mixed gas, and a nitrogen outlet for discharging nitrogen gas or nitrogen-hydrogen mixed gas that is installed in the crushing process unit,
The nitriding reaction unit includes a nitriding synthesis furnace for synthesizing the metal raw material in a nitrogen atmosphere and a nitriding synthesis control device for controlling the nitriding synthesis of the metal raw material according to the set nitriding reaction conditions.
The pulverization process unit includes a pulverization apparatus for pulverizing the nitrided raw material nitride and a mesh for sieving the pulverized raw material nitride, and includes a product entrance for entering and exiting the product, and from the pulverization process to the nitriding reaction unit or the nitriding reaction. And a moving device for moving the metal raw material or the nitrided raw material nitride through the inside of the connecting pipe from the crushing process unit to the raw material nitride in-line production apparatus for LED red phosphors. 제 11항에 있어서,
상기 연결관의 지름이 20cm인 것을 특징으로 하는 LED 적색형광체용 원료질화물 In-line화 제조장치. 12. The method of claim 11,
Raw material nitride in-line production apparatus for LED red phosphor, characterized in that the diameter of the connector 20cm.
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