Solid-State Synthesis of High Voltage Cathode Active Material: Taguchi Optimization of Ball Milling and Structural Impact of Boron Doping

Öz

The cost-performance trade-off is a critical factor in developing new cathode materials. Lithium nickel manganese oxide (LNMO) a high-voltage, cobalt-free and low-nickel chemistry, offers a promising solution in this context. In this study, boron doped micron-sized spinel LNMO is synthesized via solid-state ball milling, by optimizing milling parameters via L9 (34) Taguchi design. The effects of 1% boron doping and calcination temperature (800 and 900 °C) on the structural stability and electrochemical performance of the material are investigated. For the sample prepared at 400 rpm with a 5:1 BPR for 12 hours and calcined at 800 °C, an initial charge capacity of 110 mAh g⁻¹ is retained at 97.5 mAh g⁻¹ after 130 cycles at 0.1C. The superior capacity retention is attributed to the strengthened B–O bonding, which enhances structural stability, while calcination at 800 °C effectively minimizes particle agglomeration and facilitates the phase transformation. These results demonstrate the synergistic effects of processing optimization and boron doping on LNMO cathode performance, offering valuable insights for the advancement of lithium-ion electrode active materials.

Anahtar Kelimeler

• Spinel LNMO
• boron doping
• solid state synthesis
• high voltage cathode
• lithium-ion batteries.

Destekleyen Kurum

ITU Scientific Research Project

Proje Numarası

45208

Etik Beyan

This research does not involve human participants or animals. The authors confirm that no ethical approval was required for this study.

Teşekkür

The authors acknowledge gratefully REMER (Istanbul Medipol University) for XRD, SEM analysis. Moreover, special thanks to Metrohm for Raman.

Yüksek Voltajlı Katot Aktif Malzemesinin Katı-Hal Sentezi: Bilyalı Öğütme Proses Parametrelerinin Taguchi Yönteniyle Optimizasyonu ve Bor Katkılamasının Yapısal Etkisi

Öz

Maliyet–performans dengesi, yeni katot malzemelerinin geliştirilmesinde kritik bir faktördür. Yüksek voltajlı, kobalt içermeyen ve düşük nikel kimyasına sahip olan lityum nikel manganez oksit (LNMO), bu bağlamda umut verici bir çözüm sunmaktadır. Bu çalışmada, bor katkılanmış mikron boyutlu spinel LNMO, katı-hal bilyalı öğütme yöntemiyle sentezlenmiş; öğütme parametreleri L9 (3⁴) Taguchi deney tasarımı kullanılarak optimize edilmiştir. %1 bor katkılamasının ve kalsinasyon sıcaklığının (800 ve 900 °C) malzemenin yapısal kararlılığı ve elektrokimyasal performansı üzerindeki etkileri araştırılmıştır. 400 rpm hızda, 5:1 bilya-toz oranı (BPR) ile 12 saat öğütülen ve 800 °C’de kalsine edilen numune için, 0.1C hızında 130 çevrim sonunda başlangıç şarj kapasitesi olan 110 mAh g⁻¹ değeri 97.5 mAh g⁻¹ olarak korunmuştur. Üstün kapasite korunumu, yapısal kararlılığı artıran güçlendirilmiş B–O bağıyla ilişkilendirilirken; 800 °C’de yapılan kalsinasyonun partikül aglomerasyonunu etkin şekilde azalttığı ve faz dönüşümünü kolaylaştırdığı görülmüştür. Bu sonuçlar, proses optimizasyonu ile bor katkılamasının LNMO katot performansı üzerindeki sinerjik etkilerini ortaya koymakta ve lityum-iyon elektrot aktif malzemelerinin geliştirilmesi için değerli öngörüler sunmaktadır.

Anahtar Kelimeler

• Spinel LNMO
• bor katkılaması
• katı-hal sentezi
• yüksek voltajlı katot
• lityum-iyon piller

Proje Numarası

45208

Kaynakça

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