KR101334056B1 - Method for preparing nano-phosphor powder for optical conversion using co-precipication and nano-phosphor powder for optical conversion prepared by the same - Google Patents
Method for preparing nano-phosphor powder for optical conversion using co-precipication and nano-phosphor powder for optical conversion prepared by the same Download PDFInfo
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Abstract
본 발명은 태양전지에 적용되어 태양광 변환 효율을 개선할 수 있는 광 변환용 나노 형광 분말 및 공침법을 이용한 이의 제조방법에 관한 것으로서, 더욱 상세하게는 Y, V, Yb 및 Bi의 원천물질을 소정의 몰 비로 혼합하여 교반한 후에 암모니아수를 첨가하여 생성되는 침전물을 수득하는 일명 '공침법(co-precipitation)'으로 제조된 광 변환용 나노 형광 분말 및 그 제조방법에 관한 것이다. 본 발명의 광 변환용 나노 형광 분말을 태양전지에 적용하면 태양전지의 광 변환 효율을 개선할 수 있다. The present invention relates to a nano-fluorescent powder for light conversion that can be applied to solar cells and improve the photovoltaic conversion efficiency and a method of manufacturing the same using coprecipitation method, and more specifically, the source material of Y, V, Yb and Bi The present invention relates to a nano-fluorescent powder for light conversion prepared by a so-called 'co-precipitation' to obtain a precipitate produced by mixing and stirring a predetermined molar ratio and then adding ammonia water. Application of the nano-fluorescent powder for photoconversion of the present invention to a solar cell can improve the photoconversion efficiency of the solar cell.
Description
본 발명은 공침법을 이용한 광 변환용 나노 형광분말의 제조방법 및 이에 의해 제조된 광 변환용 나노 형광분말에 관한 것으로서, 더욱 상세하게는 태양전지에 적용되어 태양광 변환 효율을 개선할 수 있는 광 변환용 나노 형광 분말 및 공침법을 이용한 이의 제조방법에 관한 것이다. The present invention relates to a method for manufacturing a nano-fluorescence powder for light conversion using the coprecipitation method and to a nano-fluorescence powder for light conversion produced by the same, more specifically, can be applied to a solar cell to improve the light conversion efficiency The present invention relates to a nano fluorescent powder for conversion and a preparation method thereof using the coprecipitation method.
현재까지 태양전지용 하방 광 변환 형광소재로서 특별히 보고된 바는 없다. 현재 형광체는 대부분 형광등이나 전자디스플레이기에서 사용되고 있을 뿐이다. 예컨대, 국제공개공보 제2004-065324호를 참조할 수 있다. 그러나 이들 형광체는 흡수파장이 짧은 자외선에 맞추어져 있어서 태양광선을 잘 흡수하기에는 알맞지 않고, 흡수 대역도 대단히 좁다. 수은이나 크세논 등이 전기방전으로 발생하는 파장은 254 ㎚ 등으로 단자외선 영역에 속한다. 이는 태양광의 자외선 영역인 300∼400 ㎚의 영역과는 전혀 일치하지 않는다.Until now, there is no report as a downlight conversion fluorescent material for solar cells. Currently, phosphors are mostly used in fluorescent lamps or electronic displays. See, for example, International Publication No. 2004-065324. However, these phosphors are suited to ultraviolet rays having a short absorption wavelength, which is not suitable for absorbing sunlight, and the absorption band is also very narrow. The wavelength of mercury, xenon, and the like generated by electric discharge is 254 nm and belongs to the terminal ultraviolet region. This does not coincide at all with the 300-400 nm region which is the ultraviolet region of sunlight.
또한, 태양전지용 하방 광 변환 형광소재로 사용하기 위해서는 발광특성도 광폭이 크면서 가시광선 영역에 있어야 하나, 기존의 형광체는 적색, 녹색, 청색 중 한 파장만 강하게 나오게 되어 있다. 따라서 종래 보고된 형광체를 태양전지에 적용하는 것은 불가능하고, 효과도 없다.In addition, in order to be used as a downlight conversion fluorescent material for solar cells, the light emission characteristics should be in the visible light region with a large width, but the existing phosphor has only one wavelength of red, green, and blue. Therefore, it is impossible to apply the previously reported phosphor to a solar cell, and there is no effect.
태양전지용 하방 광 변환 형광체는 300∼470 ㎚ 범위의 넓은 영역의 자외선과 청색의 파장을 잘 흡수하여, 이 형광막을 통과한 후에는 약 470∼1000 ㎚ 범위의 영역까지 넓고 강한 장파장을 발생하여야 한다.The downlight conversion phosphor for solar cells absorbs a wide range of ultraviolet and blue wavelengths in the range of 300 to 470 nm, and after passing through the fluorescent film, it must generate a wide and strong long wavelength to the range of about 470 to 1000 nm.
본 발명의 목적은 이러한 조건을 최대한 만족하는 태양전지용 광변환 재료 및 그 제조방법을 제공하고자 하는 것이다.An object of the present invention is to provide a photovoltaic material for solar cells and a method of manufacturing the same that satisfies the above conditions.
상기 목적을 달성하기 위해, 본 발명은 In order to achieve the above object,
(S1) 산화이트리움, 산화이터비움 및 산화비스무스를 산성 용액에 용해시켜 혼합 용액을 제조하는 단계;(S1) dissolving yttrium oxide, ytterbium oxide and bismuth oxide in an acidic solution to prepare a mixed solution;
(S2) 상기 혼합 용액에 비이온수 및 암모늄메타바나테이트를 첨가하는 단계;(S2) adding non-ionized water and ammonium metavanatate to the mixed solution;
(S3) 상기 S2 단계에서 제조한 용액에 분산제 및 비이온수를 첨가하는 단계;(S3) adding a dispersant and non-ionized water to the solution prepared in step S2;
(S4) 암모니아수를 첨가하여 침전물을 형성하는 단계;(S4) adding ammonia water to form a precipitate;
(S5) 상기 침전물을 여과하여 세척 및 건조하는 단계; 및(S5) washing and drying the precipitate by filtration; And
(S6) 상기 S5 단계의 생성물을 소성하는 단계를 포함하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법을 제공한다.(S6) Provides a method for producing a nano-fluorescence powder for light conversion using the coprecipitation method comprising the step of firing the product of the step S5.
또한, 본 발명은 하기 화학식 1로 표시되는 광 변환용 나노 형광분말을 제공한다.The present invention also provides a nano-fluorescence powder for light conversion represented by the following formula (1).
[화학식 1][Formula 1]
Y1-x-yVO4:Ybx,Biy Y 1-xy VO 4 : Yb x , Bi y
(상기 화학식 1에서, 0.01≤x≤0.2이고, y는 0.03임) (In Formula 1, 0.01≤x≤0.2, y is 0.03)
본 발명의 광 변환용 나노 형광분말은 태양전지에서 버려지는 300 ㎚의 자외선에서 450 ㎚의 청색영역까지 광을 넓게 흡수하여서 470∼750 ㎚의 영역과 900∼1050 ㎚의 영역까지 2중으로 발광하는 우수한 광 특성이 있다. 본 발명의 광 변환용 나노 형광분말을 태양전지에 적용하면 전지 효율을 향상시킬 수 있다. The nano-fluorescent powder for light conversion of the present invention absorbs light widely from 300 nm ultraviolet rays discarded from solar cells to 450 nm blue region, thereby excellently emitting double light to 470 to 750 nm and 900 to 1050 nm. There is a light characteristic. Application of the nano-fluorescent powder for light conversion of the present invention to a solar cell can improve battery efficiency.
또한, 공침법을 사용하는 본 발명의 제조방법에 따르면 나노 크기의 입자를 균일하게 제조할 수 있는 효과가 있다. In addition, according to the production method of the present invention using the coprecipitation method has the effect that can be uniformly produced nano-sized particles.
도 1은 본 발명의 제조방법을 개략적으로 나타낸 흐름도이다.
도 2는 실시예에서 제조한 나노 형광분말을 주사전자현미경으로 촬영한 사진이다.
도 3은 실시예에서 제조한 나노 형광분말의 광 변환 가시광 발광 특성을 측정한 결과이다.
도 4는 실시예에서 제조한 나노 형광분말의 광 변환 근적외선 발광 특성을 측정한 결과이다. 1 is a flow chart schematically showing a manufacturing method of the present invention.
Figure 2 is a photograph taken with a scanning electron microscope of the nano-fluorescent powder prepared in Example.
Figure 3 is the result of measuring the light conversion visible light emission characteristics of the nano-fluorescent powder prepared in Example.
4 is a result of measuring the light conversion near infrared light emission characteristics of the nano-fluorescent powder prepared in Example.
본 발명에서 적용된 공침법은 Y, V, Yb 및 Bi의 원천물질을 소정의 몰비로 혼합하여 교반한 후에 암모니아수를 첨가하여 생성되는 침전물을 수득하는 방법으로서, 금속 이온들의 초기 산화를 방지하여 균일하고 미세한 나노 크기의 입자를 얻을 수 있다. The coprecipitation method applied in the present invention is a method of obtaining a precipitate formed by mixing and stirring a source material of Y, V, Yb and Bi in a predetermined molar ratio, and then adding ammonia water. Fine nano sized particles can be obtained.
도 1을 참조하여, 본 발명의 제조방법을 단계별로 더욱 상세하게 설명한다. 본 발명의 제조방법은 총 6 단계로 수행될 수 있다.
Referring to Figure 1, the manufacturing method of the present invention will be described in more detail step by step. The manufacturing method of the present invention can be performed in a total of six steps.
먼저, 산화이트리움, 산화이터비움 및 산화비스무스를 산성 용액에 용해시켜 혼합 용액을 제조한다(S1 단계).First, yttrium oxide, ytterbium oxide and bismuth oxide are dissolved in an acidic solution to prepare a mixed solution (step S1).
본 단계에서 사용되는 산화이트리움, 산화이터비움 및 산화비스무스의 순도는 99.9% 이상인 것이 바람직하다. 특히, 활성제로 사용되는 비스무스나 이터비움이 아주 소량 첨가되기 때문에 활성제의 효과를 극대화시키기 위해서는 순도가 높을수록 바람직하다. 이트리움은 부활성제로서 사용된다. The purity of yttrium oxide, ytterbium oxide and bismuth oxide used in this step is preferably 99.9% or more. In particular, since a very small amount of bismuth or iterium used as the active agent is added, the higher the purity is preferable to maximize the effect of the active agent. Yttrium is used as a deactivator.
구체적으로는 5∼120℃의 온도에서 산화이트리움 0.9∼1.0 몰, 산화이터비움 0.01∼0.2 몰 및 산화비스무스 0.01∼0.2 몰을 5∼200 ㎖의 산성 용액에 5∼120분간 완전히 용해시킴으로써 혼합 용액을 제조할 수 있다. 상기 온도 범위 내에서는 혼합과 용해가 잘 일어나고, 각 물질의 사용량은 형광물질에서의 활성제와 부활성제로서 최적의 함량이다. Specifically, a mixed solution is obtained by completely dissolving 0.9-1.0 mol of yttrium oxide, 0.01-0.2 mol of ytterbium oxide and 0.01-0.2 mol of bismuth oxide in a 5-200 ml acidic solution at a temperature of 5 to 120 ° C. for 5 to 120 minutes. Can be prepared. Within the above temperature range, mixing and dissolution occur well, and the amount of each substance is an optimal content as an activator and a deactivator in the fluorescent material.
본 단계에서 사용되는 산성 용액은 질산 용액, 염산 용액 및 황산 용액으로 이루어지는 군으로부터 선택되는 하나일 수 있으며, 바람직하게는 질산 용액이다. 산성 용액도 불순물이 적을수록, 즉, 순도가 높을수록 바람직하다.
The acidic solution used in this step may be one selected from the group consisting of nitric acid solution, hydrochloric acid solution and sulfuric acid solution, preferably nitric acid solution. The acidic solution is also preferably the less impurities, that is, the higher the purity.
다음으로, S1 단계에서 제조한 혼합 용액에 비이온수 및 암모늄메타바나테이트를 첨가한다(S2 단계).Next, non-ionized water and ammonium metavanatate are added to the mixed solution prepared in step S1 (step S2).
구체적으로는, S1 단계의 혼합 용액에 비이온수를 첨가하여 1.1∼5배의 부피가 되도록 희석하고, 상온에서 암모늄메타바나테이트 0.9∼1.3 몰을 첨가하여 10분∼2시간 동안 완전히 용해시킨다. 비이온수와 암모늄메타바나테이트를 첨가하여 완전히 용해시키면 투명하고 노란색을 띠는 용액을 제조할 수 있다. Specifically, the mixture is diluted to a volume of 1.1 to 5 times by adding non-ionized water to the mixed solution of the step S1, and 0.9 to 1.3 moles of ammonium metavanatate are added at room temperature to completely dissolve for 10 minutes to 2 hours. By completely dissolving non-ionized water and ammonium metavanatate, a clear, yellowish solution can be prepared.
본 단계에서 비이온수를 첨가하여 용액을 희석하는 이유는 반응속도가 빠르지 않게 천천히 일어나도록 하기 때문이다. 또한, 본 단계의 암모늄메타바나테이트는 모체물질로 사용되며, 금속산화물이 아니어서 비교적 쉽게 용해되므로 산화이트리움, 산화이터비움 및 산화비스무스보다 늦게 첨가하는 것이다.
The reason for the dilution of the solution by adding non-ionized water in this step is that the reaction rate occurs slowly so as not to be fast. In addition, the ammonium metavanadate in this step is used as a parent material, and since it is not a metal oxide, it is relatively easily dissolved, so it is added later than yttrium oxide, ytterbium oxide, and bismuth oxide.
이후, S2 단계에서 제조한 용액에 분산제 및 비이온수를 첨가한다(S3 단계).Thereafter, a dispersant and non-ionized water are added to the solution prepared in step S2 (step S3).
S2 단계에서 제조된 용액에 분산제를 첨가한 후, S2 단계 용액 부피의 1.1∼5배가 되도록 비이온수를 첨가한다. 본 단계에서 비이온수를 첨가하여 용액을 희석하는 이유는 충분한 용해반응이 서서히 일어나서 나노입자를 얻기 위함이다.After adding the dispersant to the solution prepared in step S2, non-ionized water is added so as to be 1.1 to 5 times the volume of the solution in step S2. The reason for diluting the solution by adding non-ionized water in this step is that sufficient dissolution reaction occurs slowly to obtain nanoparticles.
본 단계에서 사용되는 분산제는 균일한 나노입자 합성하기 위한 목적으로 사용되며, 에틸렌글리콜, 폴리비닐알콜 또는 폴리에틸렌옥사이드 중 하나를 사용할 수 있으며, 그중 에틸렌글리콜을 사용하는 것이 바람직하다. 또한, 분산제는 S2 단계에서 제조한 용액 부피의 20%의 양으로 첨가되는 것이 바람직한데, 그 이유는 나노입자 제조에 가장 적절한 비율이기 때문이다. The dispersant used in this step is used for the purpose of synthesizing uniform nanoparticles, one of ethylene glycol, polyvinyl alcohol or polyethylene oxide may be used, and ethylene glycol is preferable. In addition, the dispersant is preferably added in an amount of 20% of the volume of the solution prepared in the step S2, because it is the ratio most suitable for the production of nanoparticles.
S3 단계에서 제조한 용액에 암모니아수를 첨가함으로써 침전물을 형성한다(S4 단계).A precipitate is formed by adding ammonia water to the solution prepared in step S3 (step S4).
본 단계에서는 pH가 6 내지 13이 되도록 암모니아수를 첨가하고 10분 내지 150분 동안 교반하면 옅은 노랑색의 침전물이 형성된다. 본 단계에서는 용액 내 존재하는 금속 이온의 수화물이 공침법에 의해 침천되어 석출된다.
In this step, ammonia water is added so that the pH is 6 to 13 and stirred for 10 to 150 minutes to form a pale yellow precipitate. In this step, the hydrate of the metal ions present in the solution is precipitated by coprecipitation and precipitated.
이후, S4 단계에서 생성된 침전물을 여과하여 세척 및 건조하여 분말 형태의 생성물을 얻는다(S5 단계).Thereafter, the precipitate produced in step S4 is filtered, washed and dried to obtain a product in powder form (step S5).
본 단계에서는 비이온수와 에탄올 및 비이온수의 혼합물을 사용하여 3∼10회 세척을 수행하고, 20∼200℃의 온도에서 10∼60분간 건조를 수행한다. 바람직하게는, 비이온수를 사용하는 세척을 최소 2회 수행하고, 에탄올과 비이온수를 1:1 부피비로 혼합한 용액을 사용하는 세척을 최소 1회 수행한다. 에탄올과 비이온수를 1:1 부피비로 혼합한 용액을 사용하는 세척을 최소 1회 이상 수행하는 이유는 미반응물 혹은 잉여반응물을 제거하기 위함이다.
In this step, washing is performed 3 to 10 times using a mixture of non-ionized water, ethanol and non-ionized water, and drying is performed for 10 to 60 minutes at a temperature of 20 to 200 ° C. Preferably, at least two washes using non-ionized water and at least one wash using a solution of ethanol and non-ionized water in a 1: 1 volume ratio are performed. The reason for performing at least one wash using a mixture of ethanol and non-ionized water in a 1: 1 volume ratio is to remove unreacted or surplus reactants.
최종적으로, S5 단계의 생성물을 소성한다(S6 단계).Finally, the product of step S5 is calcined (step S6).
구체적으로는 1차로 300∼850℃의 온도에서 30분∼4시간 동안 공기 중 1차 열처리를 수행한 후, 850∼1400℃의 온도에서 1∼8시간 동안 전기로 내에서 2차 소성하는 것이 바람직하다. 1차 열처리를 통해 나노 결정을 제조하고, 2차 소성을 통해 활성제가 격자원자와 치환한 완전한 결정이 되도록 한다. 300℃ 미만의 온도나 850℃ 초과의 온도에서 1차 열처리시 나노결정이 잘 형성되지 않으며, 1400℃를 초과한 온도에서 2차 소성 시에는 전기에너지만 낭비할 뿐, 형광특성의 향상에는 전혀 효과가 없다.
Specifically, the first heat treatment in air for 30 minutes to 4 hours at a temperature of 300 to 850 ° C. is preferably performed first, and then calcined in an electric furnace for 1 to 8 hours at a temperature of 850 to 1400 ° C. Do. The nanocrystals are prepared by primary heat treatment, and the secondary calcination allows the active agent to be a complete crystal substituted with lattice atoms. Nanocrystals do not form well during the first heat treatment at temperatures below 300 ° C or above 850 ° C, and only waste electrical energy at the time of secondary firing at temperatures above 1400 ° C and have no effect on the improvement of fluorescence properties. There is no.
이와 같이 제조된 본 발명의 광 변환용 나노 형광분말은 하기 화학식 1로 표시될 수 있다:The nano-fluorescent powder for light conversion of the present invention prepared as described above may be represented by the following Chemical Formula 1:
[화학식 1][Formula 1]
Y1 -x- yVO4:Ybx,Biy Y 1 -x- y VO 4 : Yb x , Bi y
화학식 1에서, 0.01≤x≤0.2이고, y는 0.03이다. In Formula 1, 0.01 ≦ x ≦ 0.2 and y is 0.03.
본 발명의 광 변환용 나노 형광분말은 옅은 황색을 띠며, 300∼450 ㎚ 영역의 태양광을 흡수하여 470∼750 ㎚ 영역 및 900∼1050 ㎚ 영역에서 2중으로 발광하는 특성이 있다. 따라서 본 발명의 광 변환용 나노 형광분말을 태양전지에 적용 시 태양전지에서 실제 변환이 어려운 영역의 태양광까지 변환할 수 있으므로 태양전지의 광변환 효율을 크게 향상시킬 수 있다. The nano-fluorescent powder for light conversion of the present invention has a light yellow color, and absorbs sunlight in a 300 to 450 nm region and emits light twice in the 470 to 750 nm region and the 900 to 1050 nm region. Therefore, when the nano-fluorescent powder for photoelectric conversion of the present invention is applied to a solar cell, it is possible to convert solar light in a region where it is difficult to actually convert the solar cell, thereby greatly improving the light conversion efficiency of the solar cell.
본 발명의 광 변환용 나노 형광분말은 직경이 500∼900 ㎚일 수 있다. 상기 범위의 직경은 나노 크기 범위에 속하여 태양광을 흡수 통과하는데 유리하다.
Nano fluorescence powder for light conversion of the present invention may have a diameter of 500 ~ 900 nm. The diameters in this range fall in the nano size range and are advantageous for absorbing sunlight.
이하, 실시예를 통해 본 발명을 구체적으로 설명하지만, 이러한 실시예는 본 발명을 좀 더 명확하게 이해하기 위하여 제시되는 것일 뿐 본 발명의 범위를 제한하는 목적으로 제시하는 것은 아니며, 본 발명은 후술하는 특허청구범위의 기술적 사상의 범위 내에서 정해질 것이다.
Hereinafter, the present invention will be described in detail with reference to examples, but these examples are only presented to more clearly understand the present invention, and are not intended to limit the scope of the present invention. It will be determined within the scope of the technical spirit of the claims.
실시예 Example
고순도 산화이트리움(Y2O3, 99.9% 이상) 0.96 몰, 산화이터비움(Yb2O3, 99.9% 이상) 0.01 몰 및 산화비스무스(Bi2O3, 99.9% 이상) 0.03 몰을 50 ㎖의 질산 용액에 넣고, 50℃로 가열하면서 40분간 잘 저어 완전히 용해시켰다. 이 용액에 비이온수를 첨가하여 용액 전체 부피를 150 ㎖로 제조한 후, 고순도 암모늄 메타바나테이트(NH4VO3, 99.9% 이상) 1.0 몰을 넣고 상온에서 완전히 용해시켰다. 이때, 용액은 투명하고 노란색을 띠게 된다. 이후, 5 ㎖의 에틸렌글리콜을 첨가한 후, 비이온수를 첨가하여 30분간 잘 저어 전체 용량을 250 ㎖로 증가시켰다. pH가 9가 되도록 암모니아수를 서서히 첨가하였다. 1시간 동안 저어 얇은 노랑색의 침전물을 발생시켰다. 완전히 침전이 일어나면, 맑은 상등액을 따라내고, 남은 침전물에 비이온수 150 ㎖를 부어서 잔여 불순물을 세척하였다. 이때, 침전/세척 공정은 3회 실시하는데, 2번은 비이온수를 사용하고, 1번은 에탄올이 50% 들어간 비이온수를 사용하였다.50 ml of high purity yttrium oxide (Y 2 O 3 , 99.9% or more), 0.96 mol, ytterbium oxide (Yb 2 O 3 , 99.9% or more) and bismuth oxide (Bi 2 O 3 , 99.9% or more) 0.03 mol It was put in nitric acid solution of, and stirred well for 40 minutes while heating to 50 ° C to completely dissolve. After adding non-ionized water to the solution to prepare a total volume of 150 ml, 1.0 mol of high-purity ammonium metavanatate (NH 4 VO 3 , 99.9% or more) was added thereto and completely dissolved at room temperature. At this time, the solution becomes transparent and yellow. Thereafter, 5 ml of ethylene glycol was added, followed by stirring well for 30 minutes by adding non-ionized water to increase the total capacity to 250 ml. Ammonia water was added slowly until the pH was 9. Stir for 1 hour to generate a thin yellow precipitate. After complete precipitation, the clear supernatant was drained off and 150 ml of non-ionized water was poured into the remaining precipitate to wash off the remaining impurities. At this time, the precipitation / washing process was performed three times, twice using non-ion water, and once using non-ion water containing 50% of ethanol.
120℃의 건조 오븐에서 30분간 건조하고, 분말시료를 알루미나 도가니에 넣고, 700℃에서 2시간 동안 공기 중 1차 열처리를 하였고, 이어서 1시간 동안 전기로 온도를 1100℃로 올려서 5시간 동안 2차 소성함으로써 나노 크기의 균일한 미세 형광분말을 제조하였다.
After drying for 30 minutes in a drying oven at 120 ° C., the powder sample was placed in an alumina crucible and subjected to a first heat treatment in air at 700 ° C. for 2 hours, followed by raising the temperature of the electric furnace to 1100 ° C. for 1 hour for 2 hours. By firing, a uniform fine fluorescent powder of nano size was prepared.
시험예 1: 주사전자현미경 측정Test Example 1 Scanning Electron Microscope
주사전자현미경을 사용하여 실시예에서 제조한 나노크기의 미세 형광분말을 측정한 사진을 도 2에 나타냈다. 도 2로부터, 실시예에서 제조한 미세 형광분말이 497∼941 ㎚의 나노 크기로 제조되었음을 확인할 수 있었다.
The photo of measuring the nano-sized fine fluorescent powder prepared in Example using a scanning electron microscope is shown in FIG. From FIG. 2, it was confirmed that the fine fluorescent powder prepared in Example was prepared with a nano size of 497 to 941 nm.
시험예 2: 광변환 가시광 및 근적외선 발광 특성Test Example 2: Light conversion visible light and near infrared light emission characteristics
여기파장 365 nm의 장파장 자외선을 실시예에서 제조된 형광분말에 조사하여 발광하는 변환파장을 가시광-적외선 분광측정기로 사용하여 발광 특성을 조사하였다. 그 결과를 각각 도 3 및 도 4에 나타냈다. 도 3으로부터 실시예에서 제조한 미세 형광분말이 470∼750 ㎚의 영역에서 발광하는 특성을 확인하였고, 도 4로부터 실시예에서 제조한 미세 형광분말이 900∼1050 ㎚의 영역에서 발광하는 특성을 확인하였다. The emission wavelength was investigated by using a visible light-infrared spectrometer as a conversion wavelength which emits light by irradiating the fluorescent powder prepared in Example to a long wavelength ultraviolet ray having an excitation wavelength of 365 nm. The results are shown in FIGS. 3 and 4, respectively. 3 shows the characteristic that the micro-fluorescence powder prepared in Example emits light in the region of 470 to 750 nm, and the characteristic of the micro-fluorescence powder prepared in Example confirms the emission characteristics in the region of 900 to 1050 nm. It was.
Claims (14)
(S2) 상기 혼합 용액에 비이온수 및 암모늄메타바나테이트를 첨가하는 단계;
(S3) 상기 S2 단계에서 제조한 용액에 분산제 및 비이온수를 첨가하는 단계;
(S4) 암모니아수를 첨가하여 침전물을 형성하는 단계;
(S5) 상기 침전물을 여과하여 세척 및 건조하는 단계; 및
(S6) 상기 S5 단계의 생성물을 소성하는 단계를 포함하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. (S1) dissolving yttrium oxide, ytterbium oxide and bismuth oxide in an acidic solution to prepare a mixed solution;
(S2) adding non-ionized water and ammonium metavanatate to the mixed solution;
(S3) adding a dispersant and non-ionized water to the solution prepared in step S2;
(S4) adding ammonia water to form a precipitate;
(S5) washing and drying the precipitate by filtration; And
(S6) Method for producing a nano-fluorescent powder for light conversion using the coprecipitation method comprising the step of firing the product of the step S5.
상기 S1 단계의 산성 용액은 질산 용액, 염산 용액 및 황산 용액으로 이루어지는 군으로부터 선택되는 하나인 것을 특징으로 하는 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The acid solution of the step S1 is a method for producing a nano-fluorescent powder for light conversion, characterized in that one selected from the group consisting of nitric acid solution, hydrochloric acid solution and sulfuric acid solution.
상기 S1 단계의 산성 용액은 질산 용액인 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The acid solution of the step S1 is a method for producing a nano-fluorescence powder for light conversion using the coprecipitation method, characterized in that the nitric acid solution.
상기 S1 단계는 5∼120℃의 온도에서 산화이트리움 0.9∼1.0 몰, 산화이터비움 0.01∼0.2 몰 및 산화비스무스 0.01∼0.2 몰을 5∼200 ㎖의 산성 용액에 5∼120분간 용해시키는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The step S1 is characterized by dissolving 0.9-1.0 mol of yttrium oxide, 0.01-0.2 mol of ytterbium oxide and 0.01-0.2 mol of bismuth oxide in a 5-200 ml acidic solution at a temperature of 5 to 120 ° C. for 5 to 120 minutes. Method for producing a nano-fluorescence powder for light conversion using a coprecipitation method.
상기 S2 단계는 S1 단계의 혼합 용액에 비이온수를 첨가하여 1.1∼5배의 부피가 되도록 희석하고, 상온에서 암모늄메타바나테이트 0.9∼1.3 몰을 첨가하여 10분∼2시간 동안 완전히 용해시키는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The step S2 is diluted to a volume of 1.1 to 5 times by adding non-ionized water to the mixed solution of step S1, and 0.9 to 1.3 moles of ammonium metavanatate at room temperature to completely dissolve for 10 minutes to 2 hours. Method for producing a nano-fluorescence powder for light conversion using a coprecipitation method.
상기 S3 단계의 분산제는 에틸렌글리콜, 폴리비닐알콜 또는 폴리에틸렌옥사이드인 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The dispersing agent of step S3 is ethylene glycol, polyvinyl alcohol or a method for producing a nano-fluorescent powder for light conversion using a co-precipitation method characterized in that the polyethylene oxide.
상기 S3 단계는 S2 단계에서 제조된 용액에 분산제를 첨가한 후, S2 단계 용액 부피의 1.1∼5배가 되도록 비이온수를 첨가하는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
In the step S3, after the dispersant is added to the solution prepared in step S2, non-ionic water is added so as to be 1.1 to 5 times the volume of the S2 step solution.
상기 S4 단계는 pH가 6 내지 13이 되도록 암모니아수를 첨가하고 10분 내지 150분 동안 반응시켜 침전물을 형성하는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The step S4 is a method of producing a nano-fluorescent powder for light conversion using a coprecipitation method characterized in that the pH is added to add ammonia water to 6 to 13 and react for 10 to 150 minutes.
상기 S5 단계는 비이온수와 에탄올 및 비이온수의 혼합물을 사용하여 3∼10회 세척을 수행하고, 20∼200℃의 온도에서 10∼60분간 건조하는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The step S5 is performed for 3 to 10 times using a mixture of non-ionized water and ethanol and non-ionic water, and the light conversion nano using coprecipitation method characterized in that for 10 to 60 minutes to dry at a temperature of 20 ~ 200 ℃ Method for producing fluorescent powder.
상기 S5 단계에서, 비이온수를 사용하는 세척을 최소 2회 수행하고, 에탄올과 비이온수를 1:1 부피비로 혼합한 용액을 사용하는 세척을 최소 1회 수행하는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method of claim 9,
In the step S5, the light using the coprecipitation method characterized in that at least two washes using non-ionized water, at least one wash using a solution of ethanol and non-ionized water in a 1: 1 volume ratio. Method for producing nano-fluorescent powder for conversion.
상기 S6 단계는 1차로 300∼850℃의 온도에서 30분∼4시간 동안 공기 중 1차 열처리를 수행한 후, 850∼1400℃의 온도에서 1∼8시간 동안 전기로 내에서 2차 소성하는 것을 특징으로 하는 공침법을 이용한 광 변환용 나노 형광분말의 제조방법. The method according to claim 1,
The S6 step is to perform the first heat treatment in the air for 30 minutes to 4 hours at a temperature of 300 ~ 850 ℃ first, and then secondary baking in an electric furnace for 1 to 8 hours at a temperature of 850 ~ 1400 ℃ Method for producing a nano-fluorescent powder for light conversion using the co-precipitation method characterized in that.
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| JP2017088800A (en) | 2015-11-16 | 2017-05-25 | サムスン エレクトロニクス カンパニー リミテッド | Phosphor and method for producing the same |
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| JP2008189761A (en) | 2007-02-02 | 2008-08-21 | Keio Gijuku | Method for producing fine phosphor |
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| JP2008189761A (en) | 2007-02-02 | 2008-08-21 | Keio Gijuku | Method for producing fine phosphor |
Non-Patent Citations (3)
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| Acta Phys. -Chim. Sin. 2011, 27 (10), 2427-2431 * |
| JOURNAL OF APPLIED PHYSICS 109, p 113526 (2011) * |
| Journal of Nanoscience and Nanotechnology Vol. 11, 9484-9488, 2011 * |
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