Microintergrowths of titaniferous spinel and ilmenite have been experi
mentally produced in the system Fe-Ti-Cr-O by annealing in vacuo at co
nstant temperatures in the range 700-1100 degrees C of spinel + ilmeni
te assemblages previously synthesized at 1300 degrees C under controll
ed low f(O2). Depending on the original f(O2) of synthesis at 1300 deg
rees C, annealing produces three types of microintergrowths: Type I (l
owest f(O2): 10(-11)) has rims and trellis-like lamellae of ilmenite a
s well as small blebs of metallic iron; type II (f(O2): 10(-10)-10(-9)
) shows spinel with rims and a few lamellae of ilmenite; type III (hig
hest f(O2): 10(-8.5)) displays both spinel with rims and lamellae of i
lmenite and ilmenite with rims and lamellae of spinel. On the basis of
microprobe analysis, including precise determination of the O content
s, it is shown that the synthetic microintergrowths did not form by a
redox process. Rather, the textures represent exsolution caused by vac
ancy relaxation in spinel (and, for the most reduced samples, in ilmen
ite), according to the substitution scheme Fe(2)(2+)Ti(-1)(4+)square(-
1) (1). The presence of metallic iron in the most reduced samples (typ
e I) results from the shift of the iron saturation surface toward more
Fe-rich compositions with decreasing temperature. The rims and lamell
ae of spinel around and within ilmenite in the type-III samples result
from the combination of Exchange 1 and the well-known substitution Fe
2+ + Ti4+ = 2Fe(3+). These experimental results show that natural spin
el + ilmenite microintergrowths do not always result from either an ox
idation or a reduction process. In particular, textures similar to tho
se of type I, which were observed in lunar basalts, may simply record
cooling under O-2-conserving conditions. In most terrestrial rocks, ho
wever, spinel + ilmenite intergrowths are certainly best interpreted a
s resulting from oxidation of at least a subsystem of the rock.