CN104953023A - Preparation method of high-density Fe(Se,Te) superconducting material - Google Patents
Preparation method of high-density Fe(Se,Te) superconducting material Download PDFInfo
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- 229910052714 tellurium Inorganic materials 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 161
- 239000011669 selenium Substances 0.000 claims abstract description 126
- 239000011812 mixed powder Substances 0.000 claims abstract description 97
- 238000000713 high-energy ball milling Methods 0.000 claims abstract description 91
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 81
- 238000005245 sintering Methods 0.000 claims abstract description 61
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 32
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 13
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 180
- 230000008569 process Effects 0.000 claims description 152
- 239000002887 superconductor Substances 0.000 claims description 68
- 238000000227 grinding Methods 0.000 claims description 64
- 229910001220 stainless steel Inorganic materials 0.000 claims description 40
- 239000010935 stainless steel Substances 0.000 claims description 40
- 239000003708 ampul Substances 0.000 claims description 30
- 239000011261 inert gas Substances 0.000 claims description 30
- 239000010453 quartz Substances 0.000 claims description 30
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- 239000000758 substrate Substances 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000009702 powder compression Methods 0.000 claims description 10
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- 229910052786 argon Inorganic materials 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- 238000007906 compression Methods 0.000 claims description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 abstract description 19
- 238000000498 ball milling Methods 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 abstract 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
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- 229910018110 Se—Te Inorganic materials 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-density Fe(Se,Te) superconducting material. The method comprises steps as follows: step one, ferrous powder, selenium powder and tellurium powder are mixed to form mixed powder, and the mixed powder is placed in a vacuum ball milling tank; step two, the mixed powder is subjected to high-energy ball milling; step three, the mixed powder is pressed, and a Fe(Se,Te) green body is obtained; step four, the Fe(Se,Te) green body is sintered, and the Fe(Se,Te) superconducting material is obtained. The mole ratio of the ferrous powder to the selenium powder to the tellurium powder in the mixed powder is adjusted and controlled, the Fe content in the generated tetragonal phase Fe(Se, Te) is optimized, the mixed powder is subjected to high-energy ball milling in shorter time by means of a high-energy ball mill, limit to the reaction rate in the diffusion process during sintering is eliminated, holes formed after melting of the selenium powder are avoided, and the high-density Fe(Se,Te) superconducting material with high superconducting phase content is obtained.
Description
Technical field
The invention belongs to superconductor preparing technical field, be specifically related to a kind of preparation method of high density Fe (Se, Te) superconductor.
Background technology
2008, Japanese Hosono seminar found the LaO with 26K critical temperature
1-xf
xfeAs iron-based high-temperature superconductive material, Fe base high temperature super conductive material (FHTS) development subsequently rapidly.At present, can be divided into four Main Systems by barrier layer difference, be " 1111 " system (as LaFeAsOF) respectively, " 122 " system is (as BaFe
2as
2), " 111 " system (as LiFeAs) and " 11 " system (as FeSe).Similar with high temperature copper oxide superconductor (CHTS), the crystal structure of FHTS is all layer structure, by-FeAs-layer (or-FeSe-layer) as superconducting layer.
The main cause that FHTS develops rapidly has, and first, it is generally acknowledged that the magnetic of Fe has destruction to the electron pairing in conventional superconductor, therefore in FHTS, and coexisting of magnetic and superconductivity provides new way for exploring superconducting mechanism; Secondly, FHTS has higher superconductivity, and anisotropy is weak, is applicable to the needs of practical application, and the upper critical field (Hc of FHTS
2) far above Metal Substrate low temperature superconducting material, as Nb
3sn, NbTi and MgB
2deng, general FHTS is Hc when about 4.2K
2can reach more than 50T, be Nb
3sn (Hc
2for 30T) twice about, and Sr
0.6k
0.4fe
2as
2hc
2reach about 140T especially, the decay of the current-carrying performance of FHTS under magnetic field is simultaneously comparatively slow, even under the magnetic field condition of 20T, the critical current density (Jc) of many FHTS also can reach 10
5a/cm
-2above; In addition, the Jc of FHTS is higher, if SmFeAsOF monocrystalline is 2 × 10 at the Jc of 5K
6a/cm
-2, Ba
0.6k
0.4fe
2a
2monocrystalline Jc when 4.2K is 4 × 10
5a/cm
-2, FeTe
0.61se
0.39jc can 1 × 10 be reached lower than during its critical temperature 14K
5a/cm
-2, these performance guarantees possibility of FHTS practical application.In numerous FHTS, although the critical transition temperature of FeSe base superconductor is lower, under liquid helium temperature, its critical current density can reach the requirement of application, and, its raw material non precious metal, nontoxicity, deposit is abundant, makes it in commercial process, have larger advantage.Therefore, the research emphasis that the FeSe base band material with practical application potentiality is these system iron-based superconducting materials is at present prepared.Can better Fe (Se in FeSe base superconductor neutrality, Te) superconductor is the emphasis that we pay close attention to, relative to FeSe superconductor, Fe (Se, Te) critical temperature of superconductor higher (15K), critical current density is larger, therefore prepares practical most important to iron-based superconduction of Fe (Se, Te) superconductor band of good performance.
And prior art is at Fe (Se, Te) the main problem existed in superconductor preparation process is: due to Fe (Se, Te) there are two kinds of crystal structures, one is six side's phases, wherein, Fe:(Se, Te) ratio is a little less than 1:1, because the restriction six side phase Fe (Se, Te) of structure does not possess superconductivity; Another kind is Tetragonal, and in this structure ,-Fe (Se, Te)-distribution in sheet, namely becomes the superconducting layer structure similar with-CuO-to-FeAs-, therefore, at about 14K, suiperconducting transition occurs.In the sintering process of material, there is between these two kinds of structures the relation mutually transformed.At present, adopt conventional sintering method, or the raising of superconducting phase content is obtained by the method that sinters again after carrying out general milling to the precursor powder means only by improving sintering temperature and extending sintering time, sintering efficiency is poor, this method not only consumes a large amount of energy, and best content of tetragonal phase also only can reach less than 80%, and to obtain the density of sample extremely low, the low preparation of core silk density to superconducting wire brings very large negative effect, in this case, superconducting phase is difficult to reach UNICOM, the current-carrying performance of material is lower, therefore Fe (the Se of development of new is needed in prior art badly, Te) superconductor preparation method, to follow-up high performance Fe (Se, Te) exploration of superconducting wire and Fe base superconductor Superconducting Mechanism all has great importance.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned deficiency of the prior art, a kind of high density Fe (Se is provided, Te) preparation method of superconductor, when this method eliminateing sintering processes, diffusion process is to the restriction of reaction rate, and the hole caused after avoiding selenium powder fusing, obtains having high superconduction phase content and highdensity Fe (Se, Te) superconductor, the advantages such as have energy consumption little, technological process is short, and repeatability is strong.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of preparation method of high density Fe (Se, Te) superconductor, is characterized in that, comprise the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder is (0.9 ~ 1.4): x:(1-x by mol ratio) iron powder, selenium powder and tellurium powder mix, described x=0.2 ~ 0.8;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, be not less than 1500r/min at the rotating speed of high energy ball mill condition under by mixed powder high-energy ball milling process 5min ~ 30min, be soaked in liquid nitrogen after then vacuum sphere grinding jar being taken out and cool; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:(1 ~ 20);
Step 202, repetition step 201, until add up high-energy ball milling process 0.5h ~ 12h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 2min ~ 30min after high-energy ball milling process under the pressure of tablet press machine is the condition of 5MPa ~ 10MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 500 DEG C ~ 700 DEG C conditions, Te) blank sintering process 8h ~ 25h, again not to be down to room temperature higher than the rate of temperature fall of 30 DEG C/h, obtain Fe (Se, Te) superconductor; The density of described Fe (Se, Te) superconductor is not less than 5.02g/cm
3, described sintering processes is carried out in vacuum or argon gas atmosphere.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, is characterized in that, iron powder described in step one is reduced iron powder, the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, is characterized in that, the mol ratio of iron powder described in step one, selenium powder and tellurium powder is (1.0 ~ 1.2): x:(1-x), described x=0.4 ~ 0.6.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, is characterized in that, the mol ratio of described iron powder, selenium powder and tellurium powder is 1.1:0.5:0.5.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, it is characterized in that, the ratio of grinding media to material of the process of high-energy ball milling described in step 201 is 1:(3 ~ 6), in step 202, the time of accumulative high-energy ball milling process is 2h ~ 6h.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, is characterized in that, the ratio of grinding media to material of described high-energy ball milling process is 1:6, and the time of accumulative high-energy ball milling process is 4h.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, it is characterized in that, the pressure of compression process described in step 3 is 8MPa ~ 10MPa, the time of compression process is 5min ~ 20min.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, it is characterized in that, the pressure of described compression process is 10MPa, the time of compression process is 10min.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, is characterized in that, the temperature of sintering processes described in step 4 is 600 DEG C ~ 700 DEG C, and the time of sintering processes is 10h ~ 24h.
The preparation method of above-mentioned a kind of high density Fe (Se, Te) superconductor, it is characterized in that, the temperature of described sintering processes is 650 DEG C, the time of sintering processes is 15h.
The present invention compared with prior art has the following advantages:
1, the present invention adopts the technical process of high-energy ball milling assisted sintering to prepare highdensity Fe (Se, Te) superconductor, wherein, by iron powder in regulation and control mixed powder, the mol ratio of selenium powder and tellurium powder, optimize the Tetragonal Fe (Se generated, Te) iron content in, then utilize high energy ball mill that mixed powder is carried out high-energy ball milling process in the short period of time, while reducing mixed powder Primary Particle Size, obtain Fe-Se-Te ternary solid solution, make the Fe in mixed powder, Se and Te reaches the mixing of atom level, when eliminating sintering processes, diffusion process is to the restriction of reaction rate, and avoid due to iron powder skewness and generate six side phase Fe (Se, Te) hole caused after defect and selenium powder melt, again by after mixed powder compressing tablet through oversintering process, obtain that there is high superconduction phase content and highdensity superconductor, there is energy consumption little, technological process is short, the advantages such as repeatability is strong.
2, the mechanical energy produced by high-energy ball milling in the present invention makes mixed powder alloying, this mechanical alloying process can make iron powder, combination between selenium powder and tellurium powder tightr, and the fusing of selenium powder can be avoided, in sintering process, make the porosity reduce, obtain highdensity Fe (Se, Te) superconductor, and adopt traditional handicraft prepare without Te adulterate FeSe superconductor time high-energy ball milling can't affect to some extent density of material.
3, compared with preparing the method for superconductor with traditional planetary ball mill assisted sintering technique, the technique that the present invention adopts high energy ball mill to carry out high-energy ball milling process not only shortens ball milling required time (planetary ball mill needs more than 20h) greatly, avoid the defect that long-time ball milling may cause mixed powder oxidized, and reduce energy consumption, in addition, Fe after high-energy ball milling process in mixed powder, Se and Te is more evenly distributed, Tetragonal Fe (Se is obtained after sintering processes, Te) content is higher, larger relative to the density of non-milled sample, Fe (Se prepared by the present invention, Te) superconductor can meet the requirement to iron-based superconducting material purity and performance of subsequent experimental and commercial Application, be suitable for industrialization large-scale production.
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 be in the embodiment of the present invention 1 mixed powder through high-energy ball milling SEM photo before treatment.
Fig. 2 is the SEM photo of mixed powder after high-energy ball milling process in the embodiment of the present invention 1.
Fig. 3 is the XRD spectra of Fe (Se, Te) superconductor prepared by the embodiment of the present invention 1.
Fig. 4 is the superconducting transition temperature curve of Fe (Se, Te) superconductor prepared by the embodiment of the present invention 1.
Fig. 5 is the XRD spectra of Fe (Se, Te) superconductor prepared by the embodiment of the present invention 2.
Embodiment
Embodiment 1
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.1:0.5:0.5, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1740r/min by mixed powder high-energy ball milling process 10min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:6;
Step 202, repetition step 201, until add up high-energy ball milling process 4h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 10min after high-energy ball milling process under the pressure of tablet press machine is the condition of 10MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 650 DEG C of conditions, Te) blank sintering process 15h, be down to room temperature with the rate of temperature fall of 25 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Composition graphs 1 and Fig. 2 can contrast and find out, after high-energy ball milling process, the microscopic particles size of mixed-powder there occurs larger change, average particle size particle size is by more than 50 μm, less than 10 μm are reduced to, as seen from Figure 3, Fe (Se prepared by the present embodiment, Te) be Tetragonal Fe (Se, Te) structure, without dephasign, as seen from Figure 4, Fe (Se prepared by the present embodiment, Te) superconducting transition temperature (Tc) of superconductor is 11.1K, show good superconductivity, Fe (Se prepared by test the present embodiment, Te) density of superconductor is 5.61g/cm
3, and do not adopt high-energy ball milling, the density only obtaining Fe (Se, Te) superconductor through identical compacting and sintering process is 2.29g/cm
3, it can thus be appreciated that the technique of high-energy ball milling assisted sintering can improve the density of Fe (Se, the Te) superconductor of preparation greatly, lay the first stone for preparing high density superconducting tape core silk from now on.
Embodiment 2
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.2:0.5:0.5, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1800r/min by mixed powder high-energy ball milling process 20min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:6;
Step 202, repetition step 201, until add up high-energy ball milling process 2h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 20min after high-energy ball milling process under the pressure of tablet press machine is the condition of 9MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 700 DEG C of conditions, Te) blank sintering process 8h, be down to room temperature with the rate of temperature fall of 20 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in vacuum atmosphere.
As seen from Figure 5, the Fe (Se, Te) that prepared by the present embodiment is Tetragonal Fe (Se, Te) structure, without dephasign, Fe (Se prepared by the present embodiment, Te) superconducting transition temperature (Tc) of superconductor is 10.1K, and density is 5.61g/cm
3, there is high density and good superconductivity.
Embodiment 3
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.0:0.3:0.7, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1500r/min by mixed powder high-energy ball milling process 30min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:10;
Step 202, repetition step 201, until add up high-energy ball milling process 8h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 30min after high-energy ball milling process under the pressure of tablet press machine is the condition of 10MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 600 DEG C of conditions, Te) blank sintering process 10h, be down to room temperature with the rate of temperature fall of 15 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 90vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 10.5K, and density is 5.65g/cm
3, there is high density and good superconductivity.
Embodiment 4
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.4:0.6:0.4, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1700r/min by mixed powder high-energy ball milling process 20min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:3;
Step 202, repetition step 201, until add up high-energy ball milling process 6h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 10min after high-energy ball milling process under the pressure of tablet press machine is the condition of 8MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 500 DEG C of conditions, Te) blank sintering process 25h, be down to room temperature with the rate of temperature fall of 15 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 95vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 9.2K, and density is 5.63g/cm
3, there is high density and good superconductivity.
Embodiment 5
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 0.9:0.4:0.6, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 2000r/min by mixed powder high-energy ball milling process 5min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:4;
Step 202, repetition step 201, until add up high-energy ball milling process 0.5h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 2min after high-energy ball milling process under the pressure of tablet press machine is the condition of 9MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 650 DEG C of conditions, Te) blank sintering process 16h, be down to room temperature with the rate of temperature fall of 16 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 90vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 8.1K, and density is 5.02g/cm
3, there is high density and good superconductivity.
Embodiment 6
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.1:0.2:0.8, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1600r/min by mixed powder high-energy ball milling process 25min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:20;
Step 202, repetition step 201, until add up high-energy ball milling process 12h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 15min after high-energy ball milling process under the pressure of tablet press machine is the condition of 5MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 550 DEG C of conditions, Te) blank sintering process 20h, be down to room temperature with the rate of temperature fall of 20 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 92vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 10.8K, and density is 5.66g/cm
3, there is high density and good superconductivity.
Embodiment 7
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.0:0.8:0.2, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 1650r/min by mixed powder high-energy ball milling process 15min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:1;
Step 202, repetition step 201, until add up high-energy ball milling process 10h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 25min after high-energy ball milling process under the pressure of tablet press machine is the condition of 6MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 680 DEG C of conditions, Te) blank sintering process 13h, be down to room temperature with the rate of temperature fall of 25 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 93vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 9.8K, and density is 5.54g/cm
3, there is high density and good superconductivity.
Embodiment 8
The present embodiment comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder by mol ratio be the iron powder of 1.2:0.7:0.3, selenium powder and tellurium powder mix; Described iron powder is reduced iron powder, and the quality purity of described iron powder is not less than 99%, and the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, under the rotating speed of high energy ball mill is the condition of 2000r/min by mixed powder high-energy ball milling process 10min, be soaked in liquid nitrogen and cool after then vacuum sphere grinding jar being taken out; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:4.5;
Step 202, repetition step 201, until add up high-energy ball milling process 4h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 5min after high-energy ball milling process under the pressure of tablet press machine is the condition of 10MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 620 DEG C of conditions, Te) blank sintering process 18h, be down to room temperature with the rate of temperature fall of 15 DEG C/h again, obtain Fe (Se, Te) superconductor; Described sintering processes is carried out in argon gas atmosphere.
Fe (Se prepared by the present embodiment, Te) principal phase is Tetragonal Fe (Se, Te) structure, and Tetragonal Fe (Se, Te) content reaches 93vol%, the superconducting transition temperature (Tc) of Fe (Se, Te) superconductor prepared by the present embodiment is 8.9K, and density is 5.33g/cm
3, there is high density and good superconductivity.
The above; it is only preferred embodiment of the present invention; not the present invention is imposed any restrictions, every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection range of technical solution of the present invention.
Claims (10)
1. a preparation method for high density Fe (Se, Te) superconductor, is characterized in that, comprises the following steps:
Step one, in the glove box being full of inert gas, mixed powder is placed in vacuum sphere grinding jar, then takes out after the sealing of vacuum sphere grinding jar; Described mixed powder is (0.9 ~ 1.4): x:(1-x by mol ratio) iron powder, selenium powder and tellurium powder mix, described x=0.2 ~ 0.8;
Step 2, the vacuum sphere grinding jar that mixed powder is housed in step one is placed in high energy ball mill carries out high-energy ball milling process, detailed process is:
Step 201, be not less than 1500r/min at the rotating speed of high energy ball mill condition under by mixed powder high-energy ball milling process 5min ~ 30min, be soaked in liquid nitrogen after then vacuum sphere grinding jar being taken out and cool; In the process of described high-energy ball milling process, the temperature of mixed powder is not higher than 60 DEG C, and the ratio of grinding media to material of described high-energy ball milling process is 1:(1 ~ 20);
Step 202, repetition step 201, until add up high-energy ball milling process 0.5h ~ 12h by mixed powder;
Step 3, in the glove box being full of inert gas, mixed powder in step 2 after high-energy ball milling process is taken out from vacuum sphere grinding jar and puts into stainless steel mould, take out from glove box after stainless steel mould is sealed, then stainless steel mould is placed on tablet press machine, by the mixed powder compression process 2min ~ 30min after high-energy ball milling process under the pressure of tablet press machine is the condition of 5MPa ~ 10MPa, obtain Fe (Se, Te) base substrate;
Step 4, in the glove box being full of inert gas, by (the Se of Fe described in step 3, Te) base substrate takes out and is placed in quartz ampoule from stainless steel mould, take out from glove box after quartz ampoule is sealed, then quartz ampoule is placed in sintering furnace, to Fe (Se under the temperature of sintering furnace is 500 DEG C ~ 700 DEG C conditions, Te) blank sintering process 8h ~ 25h, again not to be down to room temperature higher than the rate of temperature fall of 30 DEG C/h, obtain Fe (Se, Te) superconductor; The density of described Fe (Se, Te) superconductor is not less than 5.02g/cm
3, described sintering processes is carried out in vacuum or argon gas atmosphere.
2. according to a kind of high density Fe (Se according to claim 1, Te) preparation method of superconductor, it is characterized in that, iron powder described in step one is reduced iron powder, the quality purity of described iron powder is not less than 99%, the quality purity of described selenium powder is not less than 99%, and the quality purity of described tellurium powder is not less than 99%.
3. according to a kind of high density Fe (Se according to claim 1, Te) preparation method of superconductor, it is characterized in that, the mol ratio of iron powder described in step one, selenium powder and tellurium powder is (1.0 ~ 1.2): x:(1-x), described x=0.4 ~ 0.6.
4. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 3, it is characterized in that, the mol ratio of described iron powder, selenium powder and tellurium powder is 1.1:0.5:0.5.
5. according to a kind of high density Fe (Se according to claim 1, Te) preparation method of superconductor, it is characterized in that, the ratio of grinding media to material of the process of high-energy ball milling described in step 201 is 1:(3 ~ 6), in step 202, the time of accumulative high-energy ball milling process is 2h ~ 6h.
6. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 5, it is characterized in that, the ratio of grinding media to material of described high-energy ball milling process is 1:6, and the time of accumulative high-energy ball milling process is 4h.
7. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 1, it is characterized in that, the pressure of compression process described in step 3 is 8MPa ~ 10MPa, and the time of compression process is 5min ~ 20min.
8. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 7, it is characterized in that, the pressure of described compression process is 10MPa, and the time of compression process is 10min.
9. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 1, it is characterized in that, the temperature of sintering processes described in step 4 is 600 DEG C ~ 700 DEG C, and the time of sintering processes is 10h ~ 24h.
10. according to the preparation method of a kind of high density Fe (Se, Te) superconductor according to claim 9, it is characterized in that, the temperature of described sintering processes is 650 DEG C, and the time of sintering processes is 15h.
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| CN108467271A (en) * | 2018-05-16 | 2018-08-31 | 天津大学 | A method of improving superconducting phase content in FeSe bulks |
| CN108467271B (en) * | 2018-05-16 | 2021-03-16 | 天津大学 | Method for increasing superconducting phase content in FeSe bulk |
| CN112863761B (en) * | 2021-02-10 | 2022-04-01 | 上海交通大学 | Iron-selenium-tellurium superconducting material and preparation method thereof |
| CN112863761A (en) * | 2021-02-10 | 2021-05-28 | 上海交通大学 | Iron-selenium-tellurium superconducting material and preparation method thereof |
| CN113345640B (en) * | 2021-06-03 | 2022-08-02 | 西北有色金属研究院 | Preparation method of Fe (Se, Te) superconducting wire |
| CN113345640A (en) * | 2021-06-03 | 2021-09-03 | 西北有色金属研究院 | Preparation method of Fe (Se, Te) superconducting wire |
| CN113402277A (en) * | 2021-06-16 | 2021-09-17 | 上海大学 | FeSe1-xTexPreparation process of target material |
| CN113643854A (en) * | 2021-08-24 | 2021-11-12 | 西北有色金属研究院 | Preparation method of graphene composite Fe (Se, Te) superconducting material |
| CN113643854B (en) * | 2021-08-24 | 2023-02-03 | 西北有色金属研究院 | Preparation method of graphene composite Fe (Se, te) superconducting material |
| CN114182350A (en) * | 2021-12-10 | 2022-03-15 | 福建师范大学 | Method for preparing FePbSeTe single-crystal superconducting material by suspension smelting method |
| CN114182350B (en) * | 2021-12-10 | 2023-06-06 | 福建师范大学 | Method for preparing FePbSeTe monocrystal superconducting material by suspension smelting method |
| CN114242333A (en) * | 2021-12-23 | 2022-03-25 | 上海交通大学 | Iron-selenium-tellurium-sulfur superconducting target material and preparation method and application thereof |
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