CN101307493A - Scheelite -type YCrO4 crystal and its high pressure synthesis method - Google Patents
Scheelite -type YCrO4 crystal and its high pressure synthesis method Download PDFInfo
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- CN101307493A CN101307493A CNA2008100575179A CN200810057517A CN101307493A CN 101307493 A CN101307493 A CN 101307493A CN A2008100575179 A CNA2008100575179 A CN A2008100575179A CN 200810057517 A CN200810057517 A CN 200810057517A CN 101307493 A CN101307493 A CN 101307493A
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Abstract
The invention relates to a scheelite-type YCrO4 crystal provided with special 3d electronic configuration and a high-pressure synthetic method thereof. YCrO4 has a square zircon-type crystal structure under normal pressure, and can produce single-phase zircon-type YCrO4 powder by taking corresponding nitrate as raw material and performing the heat treatment. Then the zircon-type YCrO4 powder is subject to the high-pressure treatment at an appropriate temperature, thereby synthesizing the YCrO4 crystal provided with a scheelite crystal structure. And the scheelite-type YCrO4 crystal can be well reserved under normal pressure, which contributes to the detailed research on a pressure-induced zircon-scheelite phase transformation mechanism and also ensures that the detailed characterization to physical and chemical properties of the YCrO4 crystal becomes possible at the same time.
Description
Technical field
The present invention relates to a kind of scheelite type YCrO
4Crystal and preparation method thereof particularly relates to a kind of scheelite type of synthetic under high pressure YCrO
4Crystal and under certain pressure and temperature condition, from Zircon cut YCrO
4Preparation scheelite type YCrO
4The crystalline method.
Background technology
Synthetic and the correlative Journal of Sex Research of novel material is the important research content of Condensed Matter Physics under the high pressure.The YCrO for preparing under the normal pressure-sintered condition
4Have cubic Zircon cut crystalline structure, spacer is I4
1/ amd.Zircon cut YCrO
4Compound makes atomic arrangement comparatively loose because of its lower positively charged ion coordination.Therefore, under certain impressed pressure, cubic zircon YCrO
4Tend to change into another cubic sheelite phase mutually.More attractive is that this structural phase transition is irreversible.Promptly after pressure release, sheelite can well be kept under condition of normal pressure mutually.To YCrO
4, we only studies show that under the impressed pressure of 3.0GPa, zircon begins to change mutually to sheelite mutually.But at ambient temperature, structural phase transition is just thoroughly finished when 15.1GPa.Pressure and temperature can provide phase transformation required energy to system simultaneously.Therefore, we make earnest efforts synthesizing the scheelite type YCrO of bulk under certain pressure and temperature condition
4Particularly, at YCrO
4In the compound, chromium ion has unusual+5 valencys, its magnetic has caused researchist's very big interest.In case we obtain the YCrO of bulk
4Sheelite high pressure cenotype can not only be studied the zircon-sheelite phase conversion mechanism of pressure inducement, also can to the structure of this phase and rerum natura particularly magnetic property characterize in detail.All these research contents are Condensed Matter Physics scholars, the general interested academic problem of Material Physics scholar and crystallophy scholar.
Summary of the invention
One of purpose of the present invention provides a kind of scheelite type YCrO
4Crystal, this scheelite type YCrO
4The crystalline spacer is cubic I4
1/ a, Z=4, lattice parameter is:
Wherein, this crystal is single-phase and is black crystals, belongs to antiferromagnetic isolator.
Another object of the present invention provides a kind of single-phase scheelite type YCrO
4The crystalline preparation method, this method comprises:
(1) under normal pressure, be I4 at first according to technique known blended space group
1The Zircon cut YCrO of/amd
4Crystal;
(2) with step (1) synthetic Zircon cut YCrO
4Crystal under certain pressure and temperature condition, is prepared scheelite type YCrO
4Crystal;
Wherein, described certain pressure and temperature condition is: pressure 6GPa-10GPa, 350 ℃-450 ℃ of temperature, soaking time 10-15 minute.
Single-phase scheelite type YCrO of the present invention
4Among the crystalline preparation method, before use, to the Zircon cut YCrO that obtains
4Crystal carries out 5-10 hour thermal treatment under 200-400 ℃ temperature condition in Oxygen Flow.
Single-phase scheelite type YCrO of the present invention
4Among the crystalline preparation method, concrete steps comprise:
With the Zircon cut YCrO that takes by weighing
4Crystal compressing tablet, and with behind goldleaf or the platinum foil parcel, in the agalmatolite chunk of packing into (as shown in Figure 1, wherein agalmatolite is as transmission medium, and steel ring and molybdenum sheet are as conduction material, and BN is as heat conduction and pressure transmission material, graphite furnace is as well heater), pressure is elevated to 6-10GPa gradually, after equipressure is stable, start heating unit, temperature is elevated to 350-450 ℃, under this temperature and high pressure, kept 10-15 minute simultaneously, then fully cooling, relief pressure again obtains the scheelite type YCrO of black
4Crystal.
Wherein, the speed that pressure raises is 1-2GPa/ minute, and the speed that temperature raises is 100-200 ℃/minute.
Wherein, the transmission medium in the described sample cavity is an agalmatolite.
The present invention is by the high pressure-temperature method, with the Zircon cut YCrO under the normal pressure
4Crystal is by the high pressure-temperature effect, and recurring structure changes, thereby obtained a kind of YCrO of new crystalline structure
4Crystal.
Description of drawings
Fig. 1 has shown the device synoptic diagram when sample carries out autoclaving.
Fig. 2 has shown Zircon cut YCrO of the present invention
4X-ray powder end diffracting spectrum.
Fig. 3 has shown scheelite type YCrO of the present invention
4The X-ray powder diffraction collection of illustrative plates.
Embodiment
Embodiment 1
(1) preparation Zircon cut YCrO
4
Y (NO with analytical pure (purity＞99%)
3)
36H
2O and Cr (NO
3)
39H
2O is that starting raw material prepares Zircon cut YCrO
4Accurately take by weighing equimolar parent material, mixed grinding is to even in agate mortar.Mixture after will grinding is then poured in the alumina crucible, puts into High Temperature Furnaces Heating Apparatus and heat-treats.Heat treatment process is as follows: 2 ℃/minute are raised to 160 ℃ with mixture from room temperature, are incubated 30 minutes; Be warmed up to 200 ℃ with 2 ℃/minute from 160 ℃ again, be incubated 30 minutes; Be raised to 580 ℃ with 10 ℃/minute from 200 ℃ then, be incubated 1 hour; Naturally cool to room temperature at last.At this moment, can obtain bottle-green Zircon cut YCrO
4In order to improve the degree of crystallinity of sample, also can be in Oxygen Flow sample be carried out anneal under 280 ℃ the temperature condition, annealing time got final product in 6 hours.Through X ray diffracting spectrum (referring to Fig. 2) can confirm, acquisition be Zircon cut YCrO
4Powder.Can determine that behind the structure refinement indexing structured data is as follows: spacer is cubic I4
1/ amd, Z=4, lattice parameter is:
And physical property measurement shows that this crystal is a ferromagnetic insulator, and ferromagnetic Curie temperature is about 9K.
(2) preparation scheelite type YCrO
4Crystal
Take by weighing the made Zircon cut YCrO of aforesaid method
4The about 0.3g of powdered sample is pressed into the disk that diameter is 6mm in advance with oil press.This sheet encapsulates entire sample after wrapping up with goldleaf in device as shown in Figure 1.Wherein graphite furnace is as well heater, and agalmatolite is as transmission medium.The agalmatolite chunk is put into the large press sample cavity, start oil pump, pressure is elevated to 6GPa gradually with 2GPa/ minute speed.After equipressure is stable, start heating unit, temperature is elevated to 450 ℃ with 150 ℃/minute speed.Under this temperature and high pressure, kept 10 minutes simultaneously.Behind the heat-insulation pressure keeping time up, remove heating power supply, and sample was kept 1-2 minute at 6GPa, making it abundant cooling, and then slow release pressure.At last, remove the goldleaf that originally was wrapped in above the sample, just can obtain the scheelite type YCrO of black
4Through X ray diffracting spectrum (referring to Fig. 3) can confirm, acquisition be monophasic scheelite type YCrO
4Crystal powder.Can determine that behind the structure refinement indexing structured data is as follows: spacer is cubic I4
1/ a, Z=4, lattice parameter is:
And physical property measurement shows that this crystal is antiferromagnetic isolator, and the antiferromagnetic transition temperature is about 21K.。
Embodiment 2
(1) preparation Zircon cut YCrO
4
Y (NO with analytical pure (purity＞99%)
3)
36H
2O and Cr (NO
3)
39H
2O is that starting raw material prepares Zircon cut YCrO
4Accurately take by weighing the parent material of equimolar amount, mixed grinding is to even in agate mortar.Mixture after will grinding is then poured in the alumina crucible, puts into High Temperature Furnaces Heating Apparatus and heat-treats.Heat treatment process is as follows: 2-5 ℃/minute is raised to 120-160 ℃ with mixture from room temperature, is incubated 30-60 minute; With 2-5 ℃/minute speed temperature is elevated to about 200-250 ℃ again, is incubated 30-60 minute; With 10-15 ℃/minute speed temperature is elevated to 520-600 ℃ then, insulation 1-3 hour; Naturally cool to room temperature at last.At this moment, can obtain bottle-green Zircon cut YCrO
4In order to improve the degree of crystallinity of sample, also can be in Oxygen Flow sample be carried out anneal, annealing time 6-12 hour under 200-400 ℃ the temperature condition.
(2) preparation scheelite type YCrO
4Crystal
Take by weighing the made Zircon cut YCrO of aforesaid method
4The about 0.3g of powdered sample is pressed into the disk that diameter is 4-6mm in advance with oil press.This sheet encapsulates entire sample after wrapping up with goldleaf in device as shown in Figure 1.Wherein graphite furnace is as well heater, and agalmatolite is as transmission medium.The agalmatolite chunk is put into the large press sample cavity, start oil pump, pressure is elevated to 6-10GPa gradually with 1-3GPa/ minute speed.After equipressure is stable, start heating unit, temperature is elevated to 350-450 ℃ with 100-200 ℃/minute speed.Under this temperature and high pressure, kept 10-15 minute simultaneously.Behind the heat-insulation pressure keeping time up, remove heating power supply, and sample was under high pressure kept 1-3 minute, making it abundant cooling, and then slow release pressure.At last, remove the goldleaf that originally was wrapped in above the sample, just can obtain the scheelite type YCrO of black
4
It should be noted that; above in conjunction with the embodiments technical scheme of the present invention is had been described in detail; but those skilled in the art will find apparent that; on the technical solution of the present invention basis; can carry out variations and modifications to technical scheme of the present invention, but not break away from the generalized scope of the present invention's claims required for protection.In addition, our scheelite type YCrO of obtaining
4Be expected to as solid-state scintillator, laser, and material such as photoelectron.
Claims (8)
1, a kind of scheelite type YCrO
4Crystal, its spacer are cubic I4
1/ a, Z=4, lattice parameter is:
2, crystal as claimed in claim 1 is characterized in that, described crystal is single-phase and is black, belongs to antiferromagnetic isolator.
3, a kind of monophasic scheelite type YCrO
4The crystalline preparation method is characterized in that,
With the Zircon cut YCrO that obtains under the normal pressure
4Crystal under certain pressure and temperature condition, the scheelite type YCrO for preparing
4Crystal; Wherein, described certain pressure and temperature condition are: pressure 6GPa-10GPa, 350 ℃-450 ℃ of temperature, soaking time 10-20 minute.
4, preparation method as claimed in claim 3 is characterized in that, described certain pressure and temperature condition is: pressure 6GPa-8GPa, 400 ℃-450 ℃ of temperature, soaking time 10-15 minute.
5, as claim 3 or 4 described preparation methods, it is characterized in that the Zircon cut YCrO that before using normal pressure is obtained down
4In Oxygen Flow, under 200-400 ℃ temperature condition, carry out 5-10 hour thermal treatment.
6, as claim 3 or 4 described preparation methods, it is characterized in that its concrete steps comprise: with the Zircon cut YCrO that takes by weighing
4Compressing tablet, and with behind goldleaf or the platinum foil parcel, in the agalmatolite chunk of packing into (as shown in Figure 1, wherein agalmatolite is as transmission medium, and steel ring and molybdenum sheet are as conduction material, and BN is as heat conduction and pressure transmission material, graphite furnace is as well heater), then pressure is elevated to 6-10GPa gradually, after equipressure is stable, start heating unit, temperature is elevated to 400-450 ℃, under this temperature and high pressure, kept 10-15 minute simultaneously, then fully cooling, relief pressure again obtains the single-phase scheelite type YCrO of black
4Crystal.
7, preparation method as claimed in claim 6 is characterized in that, the speed that pressure raises gradually is 1-2GPa/ minute, and the speed that temperature raises is 100-200 ℃/minute.
8, preparation method as claimed in claim 6 is characterized in that, the transmission medium in the described sample cavity is an agalmatolite.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104746128A (en) * | 2015-02-10 | 2015-07-01 | 中国科学院物理研究所 | Large-size high-pressure oxide single crystal growth method |
| CN110904497A (en) * | 2019-12-13 | 2020-03-24 | 澳门大学 | Centimeter-level chromium oxide single crystal, preparation method thereof and storage device |
| CN111892089A (en) * | 2020-07-07 | 2020-11-06 | 中国科学院广州地球化学研究所 | Novel hexagonal structure BaWO4And method for preparing the same |
-
2008
- 2008-02-02 CN CNA2008100575179A patent/CN101307493A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104746128A (en) * | 2015-02-10 | 2015-07-01 | 中国科学院物理研究所 | Large-size high-pressure oxide single crystal growth method |
| CN110904497A (en) * | 2019-12-13 | 2020-03-24 | 澳门大学 | Centimeter-level chromium oxide single crystal, preparation method thereof and storage device |
| CN110904497B (en) * | 2019-12-13 | 2021-06-11 | 澳门大学 | Centimeter-level chromium oxide single crystal, preparation method thereof and storage device |
| CN111892089A (en) * | 2020-07-07 | 2020-11-06 | 中国科学院广州地球化学研究所 | Novel hexagonal structure BaWO4And method for preparing the same |
| CN111892089B (en) * | 2020-07-07 | 2021-05-14 | 中国科学院广州地球化学研究所 | Hexagonal structure BaWO4And method for preparing the same |
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Open date: 20081119 |