CN102154700A - Perovskite chromium oxide crystal and preparation method thereof - Google Patents
Perovskite chromium oxide crystal and preparation method thereof Download PDFInfo
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- CN102154700A CN102154700A CN 201110127443 CN201110127443A CN102154700A CN 102154700 A CN102154700 A CN 102154700A CN 201110127443 CN201110127443 CN 201110127443 CN 201110127443 A CN201110127443 A CN 201110127443A CN 102154700 A CN102154700 A CN 102154700A
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Abstract
The invention discloses a perovskite chromium oxide crystal; the chemical formula of the crystal is as follows: LaxSrl-xCrO3; the LaxSrl-xCrO3 crystal is a cubic perovskite chromium crystal; the space group is Pm-3m; and the lattice constant is a=3.82A-3.86A. In order to further increase the content of Si, a high-temperature and high-pressure synthetic method is used for synthesizing perovskite chromium oxide LaxSrl-xCrO3 crystal, wherein 0(x is less than or equal to 0.5. The method provides the possibility for systematically researching the nature of series compounds and the influence of introduction of current carriers to bandwidth adjustable Mott compound SrCrO3 and also enriches materials serving as connecting materials of fuel cells and heating elements.
Description
Technical field
The present invention relates to a kind of uhligite chromated oxide La
xSr
1-xCrO
3Crystal and high pressure-temperature preparation method thereof.
Background technology
Bandwidth regulation and control type Mott compound S rCrO
3Synthetic must utilization high pressure-temperature synthetic method, SrCrO
3Have cubic perovskite structure, it is a paramagnetic metal.LaCrO
3Can be at normal pressure by the chemically sintered method preparation of standard solid state, it also has perovskite structure, is orthohormbic structure under the room temperature, changes monocline more than 540K into.LaCrO
3Below 295K, has antiferromagnetic preface, LaCrO under the room temperature
3Be semi-conductor, it can stand high temperature and at high temperature have good electroconductibility, so it can be used as the connection material and the Heating element of fuel cell.Substitute the serial doped compound Sr of La with Sr
xLa
1-xCrO
3And LaCrO
3The electrode materials that equally can be used as fuel cell be connected material and Heating element etc., and its performance is more excellent.The doping of Sr is very big to the influence of series compound character, and its magnetic still is antiferromagnetic, but at the following series compound of N antiferromagnetic transition can take place twice for the compound of x＜0.25 again, twice transformation all corresponding rearranging of spin direction.But use normal pressure solid state chemistry agglomerating method the content of Sr can't be surpassed 0.5, do not have before can Sr the method that further improves of doping content.
Summary of the invention
Order of the present invention is to provide a kind of uhligite chromated oxide La
xSr
1-xCrO
3Crystal another object of the present invention is to provide the method for preparing this compound.
For achieving the above object, a kind of uhligite chromated oxide of the present invention crystal, the crystalline chemical formula is: La
xSr
1-xCrO
3, this La
xSr
1-xCrO
3Crystal is the cubic perovskite crystal, and spacer is Pm-3m, and lattice parameter is a=3.82-3.86.
Further, described La
xSr
1-xCrO
3In the crystal, 0＜x≤0.5.
A kind of above-mentioned uhligite chromated oxide crystalline preparation method is specially:
Confected materials is being full of N
2Perhaps fully grind in the inert gas atmosphere, compression moulding, put it into height and be pressed into the time of under the high pressure-temperature condition of setting, carrying out the sintering setting in the assembly block, break the sample that obtains into pieces abundant grinding and carry out pickling, can prepare monophasic La after the oven dry
xSr
1-xCrO
3Crystal.
Further, described rare gas element is He, Ne, Ar.
Further, described raw material is: purity is greater than 97% SrO, and purity is greater than 99.9% La
2O
3, CrO
2And Cr
2O
3, each proportion of raw materials is SrO:La
2O
3: CrO
2: Cr
2O
3=y (1-x): 0.5x:(1-x): 0.5x, wherein 1.05≤y≤1.1.
Further, described SrO needs excessive use, and its excessive value is the 5%-10% of former set(ting)value.
Further, described raw material grinds in glove box.
Further, described raw material is pressed into cylindrical through after grinding.
Further, described crystal synthetic pressure condition is 3GPa-8GPa, and the synthetic temperature condition is 850 ℃-1400 ℃, and the synthetic time is more than the 10min.
Further, the bake out temperature of described sample is 80 ℃-200 ℃.
The present invention utilizes High Temperature High Pressure synthetic method to synthesize uhligite chromated oxide La for the content with Sr further improves
xSr
1-xCrO
3Crystal, wherein 0＜x≤0.5.This for the character of systematic research series compound, research current carrier introducing to bandwidth regulation and control type Mott compound S rCrO
3Influence provide may, also enriched the connection material of the battery that acts as a fuel and the material of Heating element.
Description of drawings
Fig. 1 is La of the present invention
xSr
1-xCrO
3Crystalline crystalline structure synoptic diagram;
Fig. 2 is La of the present invention
xSr
1-xCrO
3The XRD figure spectrum and the indexing thereof of crystal (x=0.3);
Fig. 3 is La of the present invention
xSr
1-xCrO
3The susceptibility of crystal (x=0.15) under 1000Oe magnetic field and the relation curve of temperature;
Fig. 4 is La of the present invention
xSr
1-xCrO
3The susceptibility of crystal (x=0.2) under 1000Oe magnetic field and the relation curve of temperature;
Fig. 5 is La of the present invention
xSr
1-xCrO
3The susceptibility of crystal (x=0.3) under 1000Oe magnetic field and the relation curve of temperature;
Fig. 6 is La of the present invention
xSr
1-xCrO
3The susceptibility of crystal (x=0.4) under 1000Oe magnetic field and the relation curve of temperature.
Embodiment
A kind of uhligite chromated oxide of the present invention La
xSr
1-xCrO
3Crystal, this crystal are the cubic perovskite crystal, and spacer is Pm-3m, and lattice parameter is a=3.82-3.86, wherein 0＜x≤0.5.
The invention provides uhligite chromated oxide La
xSr
1-xCrO
3The crystalline preparation method promptly uses high pressure-temperature agglomerating method to be prepared.The step that mainly comprises is as follows: confected materials is being full of N
2Perhaps fully grind in the glove box of rare gas elementes such as He, Ne, Ar, be pressed into cylinder, cylinder is put into height be pressed into assembly block and under the high pressure-temperature condition, carry out the sintering certain hour, break the sample that obtains into pieces abundant grinding and carry out pickling, can prepare monophasic La after the oven dry
xSr
1-xCrO
3Crystal.Wherein the synthetic pressure condition is 3GPa-8GPa, and the synthetic temperature condition is 850 ℃-1400 ℃, and the synthetic time is more than the 10min.And in order to suppress CrO
2Decomposition and reduce impurity, need to use the SrO of excessive 5%-10%.Bake out temperature is 80 ℃-200 ℃.
, technical scheme of the present invention is described further to shown in Figure 6 as Fig. 1 below with reference to specific embodiment.Concrete numerical value among the embodiment is not used in the protection domain that limits claims.
Embodiment 1: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 3GPa, and temperature is to carry out high-pressure sinter 10min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 2: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 10min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 3: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 8GPa, and temperature is to carry out high-pressure sinter 10min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 4: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.05 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 10min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 5: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 10min under 850 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 6: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 10min under 1400 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 7: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 30min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 8: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 9: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 10: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 120 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 11: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.05)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.05) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 200 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.05).
Embodiment 12: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.1)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.1) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.1).
Embodiment 13: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.1)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.05 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.1) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.1).
Embodiment 14: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.15)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.15) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.15).
Embodiment 15: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.2)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.2) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.2).
Embodiment 16: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.25)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.25) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.25).
Embodiment 17: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.3)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.3) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.3).
Embodiment 18: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.35)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.35) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.35).
Embodiment 19: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.4)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.4) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.4).
Embodiment 20: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.45)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.45) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.45).
Embodiment 21: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.5)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.1 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.5) thorough mixing in being full of the glove box of Ar grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.5).
Embodiment 22: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.1)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.05 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.1) is being full of N
2Glove box in thorough mixing grind, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.1).
Embodiment 23: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.1)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.05 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.1) thorough mixing in being full of the glove box of He grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.1).
Embodiment 24: use high pressure-temperature agglomerating method to prepare La
xSr
1-xCrO
3Crystal (x=0.1)
Use purity greater than 97% SrO and purity greater than 99.9% La
2O
3, CrO
2And Cr
2O
3As raw material, be SrO:La with ratio
2O
3: CrO
2: Cr
2O
3=(1.05 (1-x): 0.5x:(1-x): 0.5x) raw material of (x=0.1) thorough mixing in being full of the glove box of Ne grinds, the abrasive material that obtains is pressed into diameter is about 2mm for the 6mm height cylinder, with behind the goldleaf parcel sample sets being contained in that height is pressed in the assembly block on the big press of cubic apparatus at pressure is 5GPa, and temperature is to carry out high-pressure sinter 60min under 1000 ℃ the condition.The sample that obtains is smashed and grind, put it in the dilute hydrochloric acid and fully soak, use filter paper filtering to fall dilute hydrochloric acid and impurity then, no longer become color up to dilute hydrochloric acid so repeatedly, the atrament that obtains is dried under 80 ℃ of conditions, can obtain monophasic La
xSr
1-xCrO
3Crystal (x=0.1).
Claims (10)
1. a uhligite chromated oxide crystal is characterized in that the crystalline chemical formula is: La
xSr
1-xCrO
3, this La
xSr
1-xCrO
3Crystal is the cubic perovskite crystal, and spacer is Pm-3m, and lattice parameter is a=3.82-3.86.
2. uhligite chromated oxide crystal as claimed in claim 1 is characterized in that described La
xSr
1-xCrO
3In the crystal, 0＜x≤0.5.
3. a uhligite chromated oxide crystalline preparation method as claimed in claim 1 is characterized in that this method is specially: confected materials is being full of N
2Perhaps fully grind in the inert gas atmosphere, compression moulding, put it into height and be pressed into the time of under the high pressure-temperature condition of setting, carrying out the sintering setting in the assembly block, break the sample that obtains into pieces abundant grinding and carry out pickling, can prepare monophasic La after the oven dry
xSr
1-xCrO
3Crystal.
4. preparation method as claimed in claim 3 is characterized in that, described rare gas element is He, Ne, Ar.
5. preparation method as claimed in claim 3 is characterized in that, described raw material is: purity is greater than 97% SrO, and purity is greater than 99.9% La
2O
3, CrO
2And Cr
2O
3, each proportion of raw materials is SrO:La
2O
3: CrO
2: Cr
2O
3=y (1-x): 0.5x:(1-x): 0.5x, wherein 1.05≤y≤1.1.
6. preparation method as claimed in claim 4 is characterized in that, described SrO needs excessive use, and its excessive value is the 5%-10% of former set(ting)value.
7. preparation method as claimed in claim 3 is characterized in that described raw material grinds in glove box.
8. preparation method as claimed in claim 3 is characterized in that, described raw material is pressed into cylindrical through after grinding.
9. preparation method as claimed in claim 3 is characterized in that, described crystal synthetic pressure condition is 3GPa-8GPa, and the synthetic temperature condition is 850 ℃-1400 ℃, and the synthetic time is more than the 10min.
10. preparation method as claimed in claim 3 is characterized in that, the bake out temperature of described sample is 80 ℃-200 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105887199A (en) * | 2016-04-20 | 2016-08-24 | 中国科学院物理研究所 | Novel compound Ca2CrO4 crystal and preparation method thereof |
| CN110904497A (en) * | 2019-12-13 | 2020-03-24 | 澳门大学 | Centimeter-level chromium oxide single crystal, preparation method thereof and storage device |
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| CN1409416A (en) * | 2001-09-20 | 2003-04-09 | 北京有色金属研究总院 | Perovskite rare earth manganese oxide giant magnetic resistance material, preparing process and its use |
| CN101307491A (en) * | 2008-02-02 | 2008-11-19 | 中国科学院物理研究所 | Sr(1-x)CaxCrO3 perovskite Mott compound and its high pressure high-temperature synthesis method |
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2011
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| CN1409416A (en) * | 2001-09-20 | 2003-04-09 | 北京有色金属研究总院 | Perovskite rare earth manganese oxide giant magnetic resistance material, preparing process and its use |
| CN101307491A (en) * | 2008-02-02 | 2008-11-19 | 中国科学院物理研究所 | Sr(1-x)CaxCrO3 perovskite Mott compound and its high pressure high-temperature synthesis method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105887199A (en) * | 2016-04-20 | 2016-08-24 | 中国科学院物理研究所 | Novel compound Ca2CrO4 crystal and preparation method thereof |
| 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 |
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Application publication date: 20110817 |