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Crystallization of the lunar magma ocean yielded a chemically unique liquid residuum named KREEP. This component is expressed as a large patch on the near side of the Moon and a possible smaller patch in the northwest portion of the Moon’s South Pole-Aitken basin on the far side. Thermal models estimate that the crystallization of the lunar magma ocean (LMO) could have spanned from 10 and 200 My, while studies of radioactive decay systems have yielded inconsistent ages for the completion of LMO crystallization covering over 160 My. Here, we show that the Moon achieved >99% crystallization at 4,429 ± 76 Ma, indicating a lunar formation age of ~4,450 Ma or possibly older. Using the¹⁷⁶Lu–¹⁷⁶Hf decay system (t_1/2= 37 Gy), we found that the initial¹⁷⁶Hf/¹⁷⁷Hf ratios of lunar zircons with varied U–Pb ages are consistent with their crystallization from a KREEP-rich reservoir with a consistently low¹⁷⁶Lu/¹⁷⁷Hf ratio of 0.0167 that emerged ~140 My after solar system formation. The previously proposed younger model age of ~4.33 Ga for the source of mare basalts (240 My after solar system formation) might reflect the timing of a large impact. Our results demonstrate that lunar magma ocean crystallization took place while the Moon was still battered by planetary embryos and planetesimals leftover from the main stage of planetary accretion. The study of Lu–Hf model ages for samples brought back from the South Pole-Aitken basin will help to assess the lateral continuity of KREEP and further understand its significance in the early history of the Moon. 

The Moon has had a complex history, with evidence of its primary crust formation obscured by later impacts. Existing U-Pb dates of >500 zircons from several locations on the lunar nearside reveal a pronounced age peak at 4.33 billion years (Ga), suggesting a major, potentially global magmatic event. However, the precision of existing geochronology is insufficient to determine whether this peak represents a brief event or a more protracted period of magmatism occurring over tens of millions of years. To improve the temporal resolution, we have analyzed Apollo 14, 15, and 17 zircons that were previously dated by ion microprobe at ~4.33 Ga using isotope dilution thermal ionization mass spectrometry. Concordant dates with sub-million-year uncertainty span ~4 million years from 4.338 to 4.334 Ga. Combined with Hf isotopic ratios and trace element concentrations, the data suggest zircon formation in a large impact melt sheet, possibly linked to the South Pole–Aitken basin. 

A synthetic laser ruby crystal (HD-LR1) is introduced as a new matrix-matched reference material for secondary ionization mass spectrometry (SIMS) analysis of oxygen isotopes in corundum. Laser fluorination isotope ratio mass spectrometry (LF-IRMS) bulk analyses of multiple mg-sized fragments are homogenous, averaging δ18O = +18.40 ± 0.14‰ (95% confidence interval, n = 23) and Δ′17O = −0.368 ± 0.005‰ (as deviation from slope 0.528 for δ′17O vs. δ′18O at 95% conf., n = 11) relative to Vienna Standard Mean Ocean Water (V-SMOW). SIMS spot analyses show homogeneous O-isotopic values at the ng-scale independent of the location in the HD-LR1 single crystal and in four different crystallographic orientations. However, sample surface topography as an artefact of polishing corundum embedded in epoxy creates excess variability in δ18O within ∼100 μm from the edges of the grains. HD-LR1 is a chemical pure crystal with only Cr as a trace component detected at 276 μg g−1 by EPMA, whereas Be, often introduced in artificial gem enhancement, is <0.002 μg g−1 based on SIMS analyses. Therefore, HD-LR1 can also be used as a reference material for Cr, or as a blank for other trace element analyses of corundum by SIMS or LA-ICP-MS. 

Asteroid Ryugu and Ivuna-type carbonaceous meteorites may have originated from the outskirts of the Solar System.