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Calibration to zero-strain state
This protocol is extracted from research article:
Evidence for a strain-tuned topological phase transition in ZrTe5
Sci Adv, Aug 9, 2019;

Procedure

One of the advantages of the three-piezo apparatus compared to direct gluing to a single piezostack is that the thermal strain is minimized. This is because the large thermal expansion of the outer two piezostacks was compensated by the expansion of the middle piezostack. However, there was still a non-negligible thermal strain resulting from the mismatch of thermal expansions between the crystal and the titanium pieces of the apparatus. Because titanium is known to have a smaller thermal expansion compared to most materials, it is expected that cooling the apparatus will impart a tensile strain to a mounted crystal. By tuning the controllable strain of the apparatus, this thermal strain can be compensated if a reference calibration is available.

A zero-strain calibration was constructed by measuring the resistance of crystals before gluing to the strain apparatus. After measuring the zero-strain resistance, crystals were glued to the apparatus and the resistance was measured while cooling from 300 to 2 K. The apparatus strain could then be adjusted to tune the strained resistance to the calibration resistance, keeping the crystal in the zero-strain state. For most crystals, we were able to track the zero-strain state of the crystal down to about 60 K. Between 60 and 300 K, crystals always had a positive gauge factor (GF) (tensile strain increased resistance). This indicates that, in this temperature range, the zero-strain state resides at higher strains compared to ϵmin. Below 60 K, two things occurred that made tracking zero-strain state difficult. The first was that the resistance sensitivity to strain became weak—the GF approached zero. This indicates that the crystal either approaches or passes through ϵmin below 60 K. The second difficulty is that the resistance of the mounted crystal measured a slightly higher value than the calibration resistance for temperatures below 60 K. This occurred even when the strained crystal was tuned to ϵmin.

The higher resistance measured on the strain apparatus compared to the unstrained crystal can be attributed to a slight aging effect in the crystals. Figure S3 (A and B) shows two ZrTe5 crystals, with the resistance versus temperature measured twice. The second measurement was performed after the crystals were left sitting in atmosphere for 18 days. Between measurements, the 2 K resistance increased 2.4 and 3.4% for each crystal. The difference in resistance between crystals is negligible above 60 K, the same approximate temperature below which we are unable to tune the strained resistance to the unstrained resistance. Because of this slight aging effect, we were unable to locate the zero-strain state of crystals glued to the apparatus at low temperatures. Figure S3C shows the resistance of a strained crystal to its unstrained resistance, measured 1 day apart. Even with only 1 day between measuring the unstrained crystal and the strained crystal, there is still a slight aging effect that prohibits tracking the zero-strain state.

To estimate the location of the zero-strain state, i.e., the absolute value of ϵmin, we performed the following experiment. Crystals were glued directly on the side wall of a single piezostack, as shown in fig. S4 (B and C). The piezostack has unusual highly anisotropic thermal expansion properties; it expands by about 0.1% along the polling direction and contracts along the transverse direction as it is cooled to liquid helium temperatures. Gluing crystals oriented parallel and perpendicular to the piezostack polling axis imparts a very different strain during cooling, mimicking scenarios where samples were glued on substrates with different thermal expansion coefficients. Tuning the piezostack voltage at 2 K adds a much smaller tunable strain (~ 0.01 to 0.02%) on top of this thermal strain. Using this tunable strain, we were able to measure a linear elastoresistance. The slope of this linear response, defined as $GF=(∆ρρ)/(∆LL)$, measures the local derivative of the nonlinear resistivity versus strain curves. A positive or negative GF indicates which side of ϵmin the thermally strained crystal resides on. As seen in fig. S4, the parallel (perpendicular) orientations measure a positive (negative) GF at 2 K. This indicates the sensitivity of the thermal strain to sample preparation and allows us to make an estimate of ϵmin. On the basis of published data for the thermal expansion of similar piezostacks and ZrTe5, cooling to 2 K strains the perpendicular glued sample by about +0.08% (39, 40). The parallel glued sample is strained even more than this. We measured GF (2 K) = −73 for the perpendicular glued sample. This indicates that the parallel glued thermal strain is between −0.04 and −0.01% with respect to ϵmin, as calibrated by the quadratic response we measured for samples in this work. Combining this with our estimate for the thermal strain, we estimated that ϵmin is at most +0.12% at 2 K. With the DFT estimate of dEG/dε~6000 meV, this estimates an upper bound of the EG in the zero-strain state of 72 meV, which is consistent with most reported values of the EG.

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# Also in the Article

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