KR102054465B1 - Method for analyzing phosphorus content in cathode materials and composition used in the same - Google Patents
Method for analyzing phosphorus content in cathode materials and composition used in the same Download PDFInfo
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Abstract
본 발명은 양극재에 함유된 인의 함량 분석 방법 및 이에 사용되는 조성물에 관한 것으로, 본 발명에 따르면 이차전지 양극재에 함유된 인(P)의 회수율을 확보함으로써 분석의 정확성을 높일 수 있는 장점이 있다. The present invention relates to a method for analyzing the content of phosphorus contained in the positive electrode material and a composition used therein. According to the present invention, it is possible to increase the accuracy of analysis by securing the recovery rate of phosphorus (P) contained in the secondary battery positive electrode material. have.
Description
본 발명은 양극재에 함유된 인(P)의 함량 분석 방법 및 이에 사용되는 조성물에 관한 것이다. The present invention relates to a method for analyzing the content of phosphorus (P) contained in the cathode material and a composition used therein.
최근 핸드폰, 하이브리드 전기자동차 등에 이차전지의 사용이 증가하면서 이차전지에 대한 연구 및 개발이 활성화되고 있다. 이러한 이차전지 양극재에 금속성분을 코팅함으로써, 양극재의 구조적 안정성을 증가시키고, 전지의 성능 특성을 향상시킬 수 있다. 이러한 이차전지의 품질을 일정하게 유지하기 위하여 양극재에 함유된 물질의 정확한 성분 분석이 중요하다. Recently, as the use of secondary batteries for mobile phones and hybrid electric vehicles has increased, research and development on secondary batteries have been activated. By coating a metal component on the secondary battery positive electrode material, structural stability of the positive electrode material can be increased, and performance characteristics of the battery can be improved. In order to maintain a constant quality of the secondary battery, it is important to accurately analyze the material contained in the cathode material.
이러한 양극재의 성분 분석을 위하여 ICP(Inductively Coupled Plasma) 분석이 많이 이용된다. ICP에서 원자화 장치에 시료가 머무르는 시간은 대개 0.05~0.5초 정도로써 순간적으로 건조 과정, 회화 과정 및 원자화 과정의 3가지 작업이 이루어져야 하는데 시료에 유기물이 다량 함유되어 있거나 금속원소가 불용성 물질을 형성하고 있을 경우, 시료의 회수율이 좋지 않기 때문에 시료 전처리는 불가피하다.Inductively Coupled Plasma (ICP) analysis is widely used for component analysis of such a cathode material. In the ICP, the residence time of the sample in the atomizer is usually about 0.05 to 0.5 seconds. There are three types of operations: instant drying, incineration, and atomization. The sample contains a large amount of organic matter or a metal element forms an insoluble matter. If present, sample pretreatment is inevitable because the recovery rate of the sample is poor.
기존의 양극재의 성분 분석에서는 주로 염산을 이용하여 양극 성분을 용해하고 코팅된 성분도 용해시켜 분석을 진행하였다. 그러나, 인 (P, phosphorus)으로 코팅한 양극재에서는 염산으로 전처리를 하여 분석을 할 경우, 인이 휘발되거나 미지의 물질을 만들어 침전되어, 정확한 분석이 불가능한 단점이 있었다.In the conventional component analysis of the cathode material, the cathode component was mainly dissolved using hydrochloric acid, and the coated component was also dissolved. However, in the positive electrode material coated with phosphorus (P, phosphorus), when analyzed by pretreatment with hydrochloric acid, phosphorus volatilized or made an unknown substance and precipitated, so that accurate analysis was impossible.
이와 관련하여, Analytical and Bioanalytical Chemistry, Volume 375, Issue 4, pp 561-566에서 단백질 시료로부터 ICP-MS에 의하여 미량의 인을 검출하는 방법으로, ICP-MS를 수행하기 전 처리로, 단백질 시료를 질산 및 과산화수소에서 변성시키는 단계를 개시하고 있으나 여전히 상기와 같은 문제점은 해결되지 못한 실정이다.In this regard, Analytical and Bioanalytical Chemistry, Volume 375, Issue 4, pp 561-566, is a method for detecting trace phosphorus by ICP-MS from protein samples. Denatured in nitric acid and hydrogen peroxide is disclosed, but the above problem is still not solved.
따라서 본 발명자들은 일반적인 양극재 및 양극재 코팅 성분 분석에서 주로 사용하는 염산 용액으로는 인(P)의 분석이 불가능한 것을 확인하여 기존의 분석법과는 다르게 시료인 인(P) 성분을 함유하는 양극재에 황산을 첨가하는 단계를 포함하는 함량 분석 방법 및 황산을 포함하는, 양극재에 함유된 인(P)을 ICP 분석하기 위한 조성물을 발명함으로써 상기 문제점을 해결하였다. Therefore, the present inventors confirmed that it is impossible to analyze phosphorus (P) with a hydrochloric acid solution mainly used in general cathode materials and cathode material coating component analysis, and thus a cathode material containing phosphorus (P) component is different from conventional analytical methods. The problem was solved by inventing a content analysis method comprising the step of adding sulfuric acid to and a composition for ICP analysis of phosphorus (P) contained in the cathode material, including sulfuric acid.
본 발명은 1) 인(P) 성분을 함유하는 양극재 시료에 황산을 첨가하여 혼합하는 단계; 및The present invention comprises the steps of: 1) adding sulfuric acid to a positive electrode material sample containing a phosphorus (P) component; And
2) 상기 1)단계의 혼합물에 대해 ICP (Inductively Coupled Plasma) 분석을 수행하는 단계를 포함하는 양극재에 함유된 인(P)의 함량 분석 방법을 제공한다.2) It provides a method for analyzing the content of phosphorus (P) contained in the cathode material comprising the step of performing the ICP (Inductively Coupled Plasma) analysis for the mixture of step 1).
또한 본 발명은 인(P) 성분을 함유하는 양극재 시료 및 황산을 포함하는, 양극재에 함유된 인(P)을 ICP 분석하기 위한 조성물을 제공한다.The present invention also provides a composition for ICP analysis of phosphorus (P) contained in the cathode material, including a cathode material sample containing phosphorus (P) component and sulfuric acid.
본 발명에 따른 분석 방법 및 조성물은, 이차전지 양극재에 포함된 인(P)의 함량 분석 시 황산을 이용함으로써, 인의 회수율을 확보하여 정확한 함량 분석을 가능하게 하는 장점이 있다.Analysis method and composition according to the present invention, by using sulfuric acid when analyzing the content of phosphorus (P) contained in the secondary battery positive electrode material, there is an advantage to enable accurate content analysis to ensure the recovery of phosphorus.
본 발명은 양극재에 함유된 인(P)의 함량 분석 방법에 대한 것이다. The present invention relates to a method for analyzing the content of phosphorus (P) contained in the cathode material.
이하 각 단계별로 상세하게 설명한다.Hereinafter, each step will be described in detail.
먼저 1) 인(P) 성분을 함유하는 양극재 시료에 황산을 첨가하여 혼합한다.First, sulfuric acid is added and mixed with the positive electrode material sample containing phosphorus (P) component.
전술한 바와 같이, 기존의 양극재의 성분 분석에서는 주로 염산을 이용하여 양극 성분을 용해하였으나, 인(P) 성분을 함유하는 양극재에서는 염산으로 전처리를 할 경우 휘발되거나, 인(P)성분을 포함하는 미지의 물질을 만들어 침전됨으로써 인(P)의 정량 분석이 불가능한 문제가 있었다. As described above, in the conventional component analysis of the positive electrode material, the positive electrode component is mainly dissolved using hydrochloric acid, but in the positive electrode material containing phosphorus (P) component, it is volatilized when pretreated with hydrochloric acid or contains a phosphorus (P) component. There was a problem that the quantitative analysis of phosphorus (P) is not possible by making an unknown substance to precipitate.
이에, 본 발명자들이 검토를 행한 결과 황산을 사용하는 경우 이러한 문제점을 해결하여 분석의 정확성을 높일 수 있다는 것을 발견하여, 인(P) 성분을 함유하는 양극재 시료에 황산을 첨가하는 단계를 추가하였다. Accordingly, the inventors have found that when sulfuric acid is used, the present inventors have found that this problem can be solved to improve the accuracy of analysis, and thus, sulfuric acid is added to the cathode material sample containing phosphorus (P). .
상기 1)단계에서, 양극재 시료와 황산을 혼합 후 반응시킬 때 황산의 양을 적절하게 유지하여야 한다. 황산을 이용하여 분석을 할 경우, 황산은 시료 내에 함유되어 있는 인(P)과 반응함으로써 인이 휘발되는 것을 억제하는 기능을 한다. 즉, 반응 종료 시까지 황산이 존재하여야 인(P)의 휘발에 의한 손실을 막을 수 있어 정확한 함량 분석이 가능하므로, 황산이 완전히 증발 제거되지 않도록 하여야 한다.In step 1), the amount of sulfuric acid must be properly maintained when reacting the cathode material sample with sulfuric acid after mixing. In the case of analysis using sulfuric acid, sulfuric acid functions to suppress the volatilization of phosphorus by reacting with phosphorus (P) contained in the sample. In other words, sulfuric acid should be present until the end of the reaction to prevent loss due to volatilization of phosphorus (P), so accurate content analysis is possible, so that sulfuric acid is not completely evaporated.
또한 황산 용액의 양이 너무 많으면, 분석 오차가 커지기 때문에 황산 용액의 양을 물리적 간섭이 적은 수준으로 감소시켜 ICP-OES로 분석 시 분석 오차를 최소화하여야 한다. 만약 황산 용액의 양을 충분히 제거하지 못할 경우에는 내부 표준물법을 사용하여 앞에서 발생할 수 있는 분석 오차를 보정하여 정확한 분석을 할 수 있다.In addition, if the amount of sulfuric acid solution is too large, the analysis error is increased, so the amount of sulfuric acid solution should be reduced to a low level of physical interference to minimize the analysis error when analyzing with ICP-OES. If the amount of sulfuric acid solution is not sufficiently removed, the internal standard method can be used to correct the analytical errors that may occur before making accurate analysis.
본 발명의 분석 방법에 의하여 황산 처리가 완료되면 잔류물이 전혀 없이 유색 투명한 액체가 된다. 따라서 인의 회수율을 확보함으로써 분석의 정확성을 높일 수 있다.When the sulfuric acid treatment is completed by the analytical method of the present invention, it becomes a colored transparent liquid without any residue. Therefore, the accuracy of the analysis can be improved by securing the recovery rate of phosphorus.
본 발명에 있어서, 상기 인(P) 성분을 함유하는 양극재 시료는 인(P) 외에 추가로, 일반적으로 양극재에 포함되는 원소를 함유할 수 있으며, 바람직하게는 리튬(Li), 망간(Mn), 니켈(Ni) 및 코발트(Co)로 이루어진 군으로부터 선택된 1종 이상의 원소를 함유할 수 있다. In the present invention, the positive electrode material sample containing the phosphorus (P) component, in addition to phosphorus (P), may further contain elements generally included in the positive electrode material, preferably lithium (Li), manganese ( Mn), nickel (Ni) and cobalt (Co) may contain one or more elements selected from the group.
또한, 상기 1)단계에서 산화제를 첨가할 수 있다. 황산 첨가 후 핫 플레이트에서 가열하여 반응시키는데, 이러한 뜨거운 상태에서 산화제를 소량씩 넣어주면서 반응을 시킬 수 있다. 그 후 양극재 시료를 상온으로 냉각시킨 다음 다시 산화제를 가하여 양극재 시료를 완전히 용해시킨다. In addition, the oxidizing agent may be added in step 1). After the addition of sulfuric acid, the reaction is carried out by heating on a hot plate. In this hot state, a small amount of oxidant may be added to the reaction. After that, the cathode material sample is cooled to room temperature, and then an oxidizing agent is added to completely dissolve the cathode material sample.
상기 산화제는 질산, 과산화수소(H2O2) 및 과염소산으로 이루어진 군으로부터 선택되는 1종 이상일 수 있고, 질산 및 과산화수소인 것이 바람직하다. The oxidizing agent may be at least one selected from the group consisting of nitric acid, hydrogen peroxide (H 2 O 2 ), and perchloric acid, preferably nitric acid and hydrogen peroxide.
마지막으로, 2) 상기 1)단계의 혼합물에 대해 ICP (Inductively Coupled Plasma) 분석을 수행한다.Finally, 2) Inductively Coupled Plasma (ICP) analysis is performed on the mixture of step 1).
상기 2)단계의 ICP 분석은 210 nm 내지 215 nm의 파장에서 수행하는 것이 바람직하다. 보다 바람직하게는 213.617nm 및 214.914nm의 2개 파장을 분석하는 것이다. ICP analysis of step 2) is preferably performed at a wavelength of 210 nm to 215 nm. More preferably, two wavelengths of 213.617 nm and 214.914 nm are analyzed.
본 발명에서 사용하는 ICP 분석 방법은 ICP-OES(Inductively Coupled Plasma-Optical Emission Spectrometer), ICP-AES(Inductively Coupled Plasma-Atomic Emission Spectrometer), ICP-MS(Inductively Coupled Plasma Mass spectrometer), ICP-AAS(Inductively Coupled Plasma-Atomic Absorption Spectrometer) 등을 이용할 수 있으며, 바람직하게는 ICP-OES를 이용하여 분석하는 것이 좋다.ICP analysis method used in the present invention is ICP-OES (Inductively Coupled Plasma-Optical Emission Spectrometer), ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometer), ICP-MS (Inductively Coupled Plasma Mass Spectrometer), ICP-AAS ( Inductively Coupled Plasma-Atomic Absorption Spectrometer) and the like may be used. Preferably, the analysis is performed using ICP-OES.
본 발명의 ICP 분석 방법에 있어서, In the ICP analysis method of the present invention,
1') 상기 1)단계와 2)단계 사이에 물로 희석하는 단계를 추가적으로 포함할 수 있으며, 상기 물은 초순수인 것이 바람직하다. 1 ') may further include diluting with water between steps 1) and 2), wherein the water is preferably ultrapure water.
상기 초순수는 본 명세서에서 3차 증류수(Deionized water)와 동일한 의미로 사용되었다. 3차 증류수란 수중의 무기 염류를 이온 교환 수지 등을 이용하여 제거한 순수한 물이다. The ultrapure water is used herein in the same sense as tertiary distilled water (Deionized water). Tertiary distilled water is pure water from which inorganic salts in water were removed using ion exchange resin or the like.
또한 본 발명은 인(P) 성분을 함유하는 양극재 시료 및 황산을 포함하는, 양극재에 함유된 인(P)을 ICP 분석하기 위한 조성물에 대한 것이다.The present invention also relates to a composition for ICP analysis of phosphorus (P) contained in the cathode material, including a cathode material sample containing phosphorus (P) component and sulfuric acid.
본 발명의 일 구현예에 있어서, In one embodiment of the invention,
상기 인(P) 성분을 함유하는 양극재 시료는 인(P) 외에 추가로, 일반적으로 양극재에 포함되는 원소를 함유할 수 있으며, 바람직하게는 리튬(Li), 망간(Mn), 니켈(Ni) 및 코발트(Co)로 이루어진 군으로부터 선택된 1종 이상의 원소를 함유할 수 있다. The positive electrode material sample containing the phosphorus (P) component may further contain elements included in the positive electrode material in addition to phosphorus (P), and preferably include lithium (Li), manganese (Mn), and nickel ( Ni) and cobalt (Co) may contain one or more elements selected from the group consisting of.
본 발명의 다른 일 구현예에 있어서, In another embodiment of the present invention,
상기 조성물은 산화제를 추가로 포함할 수 있으며, 상기 산화제는 질산, 과산화수소(H2O2) 및 과염소산으로 이루어진 군으로부터 선택되는 1종 이상인 것이 바람직하다. The composition may further comprise an oxidizing agent, the oxidizing agent is preferably at least one selected from the group consisting of nitric acid, hydrogen peroxide (H 2 O 2 ) and perchloric acid.
이하 본 발명을 비한정적인 실시예에 의해 더욱 상세하게 설명한다. 하기에 개시되는 본 발명의 실시 형태는 어디까지 예시로써, 본 발명의 범위는 이들의 실시 형태에 한정되지 않는다. 본 발명의 범위는 특허청구범위에 표시되었고, 더욱이 특허 청구범위 기록과 균등한 의미 및 범위 내에서의 모든 변경을 함유하고 있다. 또한, 이하의 실시예, 비교예에서 함유량을 나타내는 "%" 및 "부"는 특별히 언급하지 않는 한 질량 기준이다.Hereinafter, the present invention will be described in more detail with reference to non-limiting examples. Embodiment of this invention disclosed below is an illustration to the last, and the scope of the present invention is not limited to these embodiment. The scope of the invention is indicated in the appended claims, and moreover contains all modifications within the meaning and range equivalent to the claims. In addition, "%" and "part" which show content in a following example and a comparative example are a mass reference | standard unless there is particular notice.
실시예Example
실시예Example 1. ICP 분석 1. ICP Analysis
1) 시료인 인(P)을 함유하는 화합물 0.1 g을 비이커에 정확히 무게를 측정하여 진한 황산 2 mL를 첨가한 후 핫 플레이트에서 가열하여 반응시켰다. 이 때, 온도는 황산의 끓는점까지 올려 주어, 황산 백연이 관찰 가능할 때까지 반응시켰다. 1) 0.1 g of a compound containing phosphorus (P) was accurately weighed in a beaker and 2 mL of concentrated sulfuric acid was added thereto, followed by heating on a hot plate to react. At this time, the temperature was raised to the boiling point of sulfuric acid and reacted until white sulfuric acid was observed.
2) 시료를 일시적으로 핫 플레이트에서 내려 놓아, 상온으로 냉각시키며 뜨거운 상태에서 질산을 0.03 mL씩 첨가하여 반응시켰다. 질산에 의해 시료의 색이 분홍색을 띄는 것을 확인하였다. 2) The sample was temporarily lowered from the hot plate, cooled to room temperature, and reacted by adding 0.03 mL of nitric acid in a hot state. The color of the sample was confirmed to be pink by nitric acid.
3) 이후 시료의 황산 용액을 완전히 증발 건고시키지 않고 소량 남도록 하고, 이를 상온으로 냉각시킨 후 다시 진한 질산 1 mL를 첨가하고 과산화수소를 0.03 mL씩 10회 첨가하여 완전히 용해시켰다. 시료가 완전히 용해된 후 초순수로 희석하였다. 3) After the sulfuric acid solution of the sample was completely evaporated to dry without remaining, and after cooling to room temperature, 1 mL of concentrated nitric acid was added again and hydrogen peroxide was added 10 times each 0.03 mL to completely dissolve. The sample was completely dissolved and then diluted with ultrapure water.
4) ICP-OES 분석 장비(Optima series, Perkinelmer 사 제조)를 이용하여 파장이 213.617 nm 와 214.914 nm 인 조건에서 상기 실시예 1 및 비교예 1에 대한 인(P) 분석을 하였다. 동일한 측정을 4회 반복 수행한 후 그에 대한 분석 결과(평균, 상대표준편차(%))를 하기 표 1에 나타내었다.4) Phosphorus (P) analysis of Example 1 and Comparative Example 1 was carried out using an ICP-OES analyzer (Optima series, manufactured by Perkinelmer) under the conditions of 213.617 nm and 214.914 nm. After repeating the same measurement four times, the results of the analysis (mean, relative standard deviation (%)) is shown in Table 1 below.
비교예Comparative example 1. ICP 분석 1. ICP Analysis
상기 실시예 1의 1)단계에서 진한 황산 1 mL 대신 염산 1 mL를 첨가한 것을 제외하고는 실시예 1과 동일한 방법으로 ICP 분석을 하였다. 동일한 측정을 2회 반복 수행한 후 그에 대한 분석 결과를 하기 표 1에 나타내었다.In the same manner as in Example 1, except that 1 mL of hydrochloric acid was added instead of 1 mL of concentrated sulfuric acid in step 1) of Example 1, ICP analysis was performed. After performing the same measurement twice, the analysis results thereof are shown in Table 1 below.
결과
result
결과
result
상기 표 1에서 볼 수 있듯이, 황산을 사용한 실시예 1의 경우 황산을 사용하지 않은 비교예 1의 경우보다 상대표준편차(%)가 2배 이상 작았다. 즉, 황산 사용 시 정밀도 및 재현성이 높은 정량분석이 가능하였다. As can be seen in Table 1, the relative standard deviation (%) of Example 1 using sulfuric acid was two times smaller than that of Comparative Example 1 without sulfuric acid. That is, quantitative analysis with high precision and reproducibility was possible when using sulfuric acid.
Claims (11)
상기 인 성분을 함유하는 양극재 시료 및 황산을 포함하는 상기 1) 단계의 혼합물에 질산, 과산화수소(H2O2) 및 과염소산으로 이루어진 군으로부터 선택되는 1종 이상의 산화제를 첨가하여 상기 양극재 시료를 용해시키는 단계; 및
2) 상기 인 성분을 함유하는 양극재 시료 및 황산을 포함하는 1) 단계의 혼합물 및 상기 산화제를 포함하는 혼합물에 대해 ICP (Inductively Coupled Plasma) 분석을 수행하는 단계를 포함하고,
상기 1) 단계에서 상기 양극재 시료에 포함되는 인(P) 성분과 황산이 반응하여, 인의 휘발이 억제되는 양극재에 함유된 인(P)의 함량 분석 방법. 1) adding sulfuric acid to a cathode material sample containing a phosphorus (P) component and mixing;
The cathode material sample was prepared by adding at least one oxidizing agent selected from the group consisting of nitric acid, hydrogen peroxide (H 2 O 2 ), and perchloric acid to the mixture of the cathode material sample containing phosphorus and sulfuric acid. Dissolving; And
2) performing an ICP (Inductively Coupled Plasma) analysis on the mixture of step 1) comprising the cathode material sample containing phosphorus and sulfuric acid and the mixture comprising the oxidant;
Method of analyzing the content of phosphorus (P) contained in the positive electrode material in which the sulfuric acid reacts with the phosphorus (P) component contained in the positive electrode material sample in step 1).
1') 상기 1) 단계와 2) 단계 사이에 물로 희석하는 단계를 추가적으로 포함하는 것을 특징으로 하는 양극재에 함유된 인(P)의 함량 분석 방법. The method according to claim 1,
1 ') The method of analyzing the content of phosphorus (P) contained in the cathode material, characterized in that it further comprises the step of diluting with water between steps 1) and 2).
상기 인(P) 성분을 함유하는 양극재 시료는 인(P) 외에 추가로, 리튬(Li), 망간(Mn), 니켈(Ni) 및 코발트(Co)로 이루어진 군으로부터 선택된 1종 이상의 원소를 함유하는 것을 특징으로 하는 양극재에 함유된 인(P)의 함량 분석 방법. The method according to claim 1,
The positive electrode material sample containing the phosphorus (P) component may include at least one element selected from the group consisting of lithium (Li), manganese (Mn), nickel (Ni), and cobalt (Co) in addition to phosphorus (P). Method for analyzing the content of phosphorus (P) contained in the positive electrode material, characterized in that it contains.
상기 2) 단계의 ICP 분석은 210 nm 내지 215 nm의 파장에서 수행하는 것을 특징으로 하는 양극재에 함유된 인(P)의 함량 분석 방법.The method according to claim 1,
ICP analysis of step 2) is a method for analyzing the content of phosphorus (P) contained in the cathode material, characterized in that performed at a wavelength of 210 nm to 215 nm.
상기 2) 단계의 ICP 분석은 유도 결합 플라즈마-분광분석기(ICP-OES, (Inductively Coupled Plasma-Optical Emission Spectrometer)를 이용하는 것을 특징으로 하는 양극재에 함유된 인(P)의 함량 분석 방법.The method according to claim 1,
ICP analysis of step 2) is the method of analyzing the content of phosphorus (P) contained in the cathode material, characterized in that using the Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES).
Samples of cathode materials containing phosphorus (P) and at least one element selected from the group consisting of lithium (Li), manganese (Mn), nickel (Ni) and cobalt (Co), sulfuric acid, nitric acid and hydrogen peroxide (H) A composition for ICP analysis of phosphorus (P) contained in the cathode material, which comprises at least one oxidizing agent selected from the group consisting of 2 O 2 ) and perchloric acid.
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