In-Situ X-ray Diffraction Studies of the Crystallisation of VOHPO4.5H2O

Kieran Hodnett; L. O'Mahony; D. Sutton

doi:10.1016/j.cattod.2004.03.031

In-Situ X-ray Diffraction Studies of the Crystallisation of VOHPO4.5H2O

Kieran Hodnett, L. O'Mahony, D. Sutton

Retired Staff

University of Limerick

Research output: Contribution to journal › Article › peer-review

Abstract

Time resolved in situ X-ray diffraction was used to study the formation of vanadyl hydrogen phosphate hemihydrate (VOHPO₄·0.5H ₂O) in organic media. This technique has identified a new phase at early synthesis times (less than 300s) at a d-spacing of 7.5 and 3.1Å. The feature at 7.5Å shifted to 6.7Å during the first 20min of synthesis and this phase collapsed as VOHPO₄·0.5H₂O formed. Thin symmetrical platelets of 10μm×10μm dimensions were observed when samples were recovered after short synthesis times. Energy dispersive X-ray analysis indicated that these platelets contained vanadium and phosphorus. The platelets appeared to delaminate possibly associated with the strain generated when the d-spacing shifted from 7.5 to 6.7Å, from which growth of the VOHPO₄·0.5H₂O into the familiar rosette morphology occurs.

Original language	English (Ireland)
Pages (from-to)	185-189
Number of pages	5
Journal	Catalysis Today
Volume	91-92
DOIs	https://doi.org/10.1016/j.cattod.2004.03.031
Publication status	Published - 15 Jul 2004

Keywords

Crystallization
In situ X-ray diffraction
VPO

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10.1016/j.cattod.2004.03.031

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@article{eafd341066a24ba28c47ff1ad1ec3819,

title = "In-Situ X-ray Diffraction Studies of the Crystallisation of VOHPO4.5H2O",

abstract = "Time resolved in situ X-ray diffraction was used to study the formation of vanadyl hydrogen phosphate hemihydrate (VOHPO4·0.5H 2O) in organic media. This technique has identified a new phase at early synthesis times (less than 300s) at a d-spacing of 7.5 and 3.1{\AA}. The feature at 7.5{\AA} shifted to 6.7{\AA} during the first 20min of synthesis and this phase collapsed as VOHPO4·0.5H2O formed. Thin symmetrical platelets of 10μm×10μm dimensions were observed when samples were recovered after short synthesis times. Energy dispersive X-ray analysis indicated that these platelets contained vanadium and phosphorus. The platelets appeared to delaminate possibly associated with the strain generated when the d-spacing shifted from 7.5 to 6.7{\AA}, from which growth of the VOHPO4·0.5H2O into the familiar rosette morphology occurs.",

keywords = "Crystallization, In situ X-ray diffraction, VPO",

author = "Kieran Hodnett and L. O'Mahony and D. Sutton",

year = "2004",

month = jul,

day = "15",

doi = "10.1016/j.cattod.2004.03.031",

language = "English (Ireland)",

volume = "91-92",

pages = "185--189",

journal = "Catalysis Today",

issn = "0920-5861",

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TY - JOUR

T1 - In-Situ X-ray Diffraction Studies of the Crystallisation of VOHPO4.5H2O

AU - Hodnett, Kieran

AU - O'Mahony, L.

AU - Sutton, D.

PY - 2004/7/15

Y1 - 2004/7/15

N2 - Time resolved in situ X-ray diffraction was used to study the formation of vanadyl hydrogen phosphate hemihydrate (VOHPO4·0.5H 2O) in organic media. This technique has identified a new phase at early synthesis times (less than 300s) at a d-spacing of 7.5 and 3.1Å. The feature at 7.5Å shifted to 6.7Å during the first 20min of synthesis and this phase collapsed as VOHPO4·0.5H2O formed. Thin symmetrical platelets of 10μm×10μm dimensions were observed when samples were recovered after short synthesis times. Energy dispersive X-ray analysis indicated that these platelets contained vanadium and phosphorus. The platelets appeared to delaminate possibly associated with the strain generated when the d-spacing shifted from 7.5 to 6.7Å, from which growth of the VOHPO4·0.5H2O into the familiar rosette morphology occurs.

AB - Time resolved in situ X-ray diffraction was used to study the formation of vanadyl hydrogen phosphate hemihydrate (VOHPO4·0.5H 2O) in organic media. This technique has identified a new phase at early synthesis times (less than 300s) at a d-spacing of 7.5 and 3.1Å. The feature at 7.5Å shifted to 6.7Å during the first 20min of synthesis and this phase collapsed as VOHPO4·0.5H2O formed. Thin symmetrical platelets of 10μm×10μm dimensions were observed when samples were recovered after short synthesis times. Energy dispersive X-ray analysis indicated that these platelets contained vanadium and phosphorus. The platelets appeared to delaminate possibly associated with the strain generated when the d-spacing shifted from 7.5 to 6.7Å, from which growth of the VOHPO4·0.5H2O into the familiar rosette morphology occurs.

KW - Crystallization

KW - In situ X-ray diffraction

KW - VPO

UR - http://www.scopus.com/inward/record.url?scp=2942711585&partnerID=8YFLogxK

U2 - 10.1016/j.cattod.2004.03.031

DO - 10.1016/j.cattod.2004.03.031

M3 - Article

AN - SCOPUS:2942711585

SN - 0920-5861

VL - 91-92

SP - 185

EP - 189

JO - Catalysis Today

JF - Catalysis Today

ER -

In-Situ X-ray Diffraction Studies of the Crystallisation of VOHPO4.5H2O

Abstract

Keywords

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