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LK99 Synthesis attempts

Testing if LK99 is for real

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The purpose of this project was to test the claim of the superconductivity of LK-99 at room temperature. The paper (linked below) that claimed this was published at the end of July and has since caused a lot of stir in the scientific community. Since our lab had a vacuum furnace, we decided to attempt to recreate creating LK-99 and testing the claim that it has superconductive qualities ("proved with the Critical temperature (Tc), Zero-resistivity, Critical current (Ic), Critical magnetic field (Hc), and the Meissner effect" Lee, S. et al. 2023) at room temperature and ambient pressure.

https://doi.org/10.48550/arXiv.2307.12008

  • Updates on LK99

    Michael Perrone03/18/2024 at 19:32 0 comments

    For those who have been paying attention, recently there have been some positive results with diamagnetic levitation of small grains of LK99 from the original team and others in South Korea and China. This rules out an anisotropic paramagnetic effect, which makes sense considering the results we observed. NextBigFuture author Brian Wang has been doing great coverage of the ongoing developments.

    It has been shown that sulfur dopes into the ceramic and doesn't solely form copper sulfide, and it is widely assumed that this is important to the process now.

    SCTL showed that a vacuum furnace is not necessary for this synthesis. They also demonstrate that there appears to be quantum locking happening in the material, not solely diamagnetism. Even if all their samples were pure lead, it wouldn't be conductive enough for eddy currents to explain the scale of effects they demonstrate.

    From our tests, we found that quartz tubes were not really usable, because the silica diffused into the LK99 ceramic. We recommend people trying to replicate this only use alumina containers.

    With all this in mind, and with the race on to find the optimal process and composition, we will continue our LK99 experiments with an emphasis on making these experiments as easy as possible for everyone here to try and replicate. We recommend anyone trying this try it with a Tabletop Furnace. In a well ventilated area of course. I am not convinved that it is neccesary to start from elemental phosphorous or sulfur also - it should also be possible to start with phosphates, sulfates and sulfides to reduce any fume formation - some of our successful samples were made that way.

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  • 1
    LK-99 Synthesis Instructions

    Below are the instructions given by the original lab that claimed to produce the room-temperature superconductor LK-99:

    - Prepare lanarkite (Pb2SO5)

         - PbO and PbSO4 mixed uniformly in a 1:1 molar ratio

         - bake in a furnace in an alumina crucible at 725C for 24 hours

         - pulverize the white powder product (lanarkite)

    - Prepare copper phosphide (Cu3P)

         - Cu and P mixed in 3:1 molar ratios

         - bake in a furnace at 550C under vacuum for 48 hours

         - pulverize dark grey product (copper phosphide)

    - Synthesize LK-99

         - lanarkite and copper phosphide were ground together into a uniform powder

         - place in a sealed crystal tube at vacuum

         - bake in a furnace for 5-20 hours to produce LK-99

  • 2
    LK-99 Synthesis First Trial

    Below are the steps that our lab followed during the first attempt of recreating LK-99:

    - Prepare lanarkite

         - weigh out roughly 1.7g PbO and 2.3g PbSO4

         - mix until uniform in a clean beaker

         - transfer to graphite crucible coated in boron nitride and seal with lid

         - pull vacuum on the furnace

         - once at vacuum, bake at 725C for 2 hours

         - remove the crucible and grind up product in a mortar before setting aside in a labeled bag

    - Prepare copper phosphide

         - weight out roughly 3g Cu (our source was originally copper wire shavings, but we used copper powder in later test as this proved to be better for our purposes) and 0.5g of P (red phosphorus powder)

         - transfer to a glass vial with a metal cap and mix until uniform

         - close the cap tightly

         - blowtorch the sample to allow for the reaction to the place without evaporating off P

         - carefully break open the glass tube and extract the product

         - grind up the copper phosphide with a mortar and pestle

    - Synthesize LK-99

         - weigh out roughly 1.8g lanarkite and 0.05g of copper phopshide, as this will allow for the molar ratio of 1 : ~9.2 copper : lead

         - weigh out roughly 0.004g of S, as the paper initially claimed that there was a sulfur impurity not accounted for

         - mix all of these uniformly in a beaker with a clean scoopula

         - transfer to an alumina crucible and place in the furnace

         - pull vacuum on the crucible and the reactants

         - bake at 925C for roughly 6 hours

         - remove the crucible and observe the crystals

    At this point, the crystals that we had retrieved were not large enough to test for super conductivity, but we did record the interactions with one of the crystals and a magnet:

    Additionally, here is a live stream with some more information on our process:

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