Skip to content

Latest commit

 

History

History
53 lines (30 loc) · 1.7 KB

README.md

File metadata and controls

53 lines (30 loc) · 1.7 KB

Project: LK99 - replication attempt

Team:

Growth process

2nd August 2023

17:00 Copper and Phosphorus powder mixed in 3:1 ratio and putted to the oven for 2 days. T = 550 °C

3rd August 2023

7:00 We were too impatient to wait for PbSO4 delivery, so prepared some this morning. PbO dissolved in nitric acid to create aqueous lead nitrate. Then precipitate out lead sulphate by adding sodium sulfate.

8:00 PbSO4 drying in the oven.

10:00 PbSO4 goes on XRD to check correct composition (see refinement bellow)

Data analysis

4th August 2023

Data from XRD at room temperature on PbSO4 refined with Fullprof (Rietveld analysis) and Jana (Le Bail method).

  • Raw data: /data/bruker/230803_PbSO4raw.dat
  • Fullprof refinement: /analysis/PbSO4-fullprof/
  • Jana refinement: /analysis/PbSO4-jana/

Resulting lattice parameters

a b c
Rietveld 8.465(1) 5.396(1) 6.952(1)
Le Bail 8.466(1) 5.395(1) 6.952(1)

Fullprof results

Jana results

Discussion: There is clearly some impurity, but in a small amount (3 unindexed peaks around 2θ = 30°). Peak shape is not perfectly fitted, because of the big step in the data acquisition.