CN103360099B - Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers - Google Patents

Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers Download PDF

Info

Publication number
CN103360099B
CN103360099B CN201310330195.1A CN201310330195A CN103360099B CN 103360099 B CN103360099 B CN 103360099B CN 201310330195 A CN201310330195 A CN 201310330195A CN 103360099 B CN103360099 B CN 103360099B
Authority
CN
China
Prior art keywords
powder
oxide crystal
metallic oxide
powder mix
whisker
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201310330195.1A
Other languages
Chinese (zh)
Other versions
CN103360099A (en
Inventor
冯建情
徐晓燕
李成山
于泽铭
金利华
张平祥
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Northwest Institute for Non Ferrous Metal Research
Original Assignee
Northwest Institute for Non Ferrous Metal Research
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Northwest Institute for Non Ferrous Metal Research filed Critical Northwest Institute for Non Ferrous Metal Research
Priority to CN201310330195.1A priority Critical patent/CN103360099B/en
Publication of CN103360099A publication Critical patent/CN103360099A/en
Application granted granted Critical
Publication of CN103360099B publication Critical patent/CN103360099B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention provides a preparation method for a YBCO superconductive block material enhanced by metal oxide crystal whiskers. The preparation method comprises the following steps: first, mixed powders are prepared; second, powder pressed compacts are prepared; third, seed crystals are placed on the top of the pressed compacts, and then the pressed compacts are subjected to crystallization to obtain a single-domain block material; fourth, the single-domain block material is objected to oxygen diffusion to obtain a YBCO superconductive block material enhanced by metal oxide crystal whiskers. The preparation method is simple and practicable, has advantages of high efficiency and easy control of reactions, and is suitable for large scale industrial production. The prepared YBCO superconductive block material enhanced by metal oxide crystal whiskers has strong magnetic levitation force, good superconductive performance and good mechanical properties.

Description

The preparation method of the YBCO superconductive block that a kind of metallic oxide crystal whisker strengthens
Technical field
The invention belongs to superconducting material technical field, be specifically related to a kind of preparation method of YBCO superconductive block of metallic oxide crystal whisker enhancing.
Background technology
Since within 1987, finding yttrium barium copper oxide (YBCO) high-temperature superconductor, there is research work prepared by the YBCO superconductive block of practical application foreground and come into one's own always.YBCO bulk, oozing meeting formation micro-crack in oxygen and melt growth process, adds the fragility of YBCO material itself, and mechanical property is lower.YBCO superconductive block can produce magnetic field stress in the time of the environment use procedure of upfield simultaneously, in the time that stress is greater than the physical strength of superconductive block, the micro-crack of bulk inside can be expanded growth, cause superconductive block to form macrocrack, cause the significantly reduction of superconductive block performance, thereby limited the widespread use of YBCO bulk.
In order to improve the mechanical property of superconductive block, the Japan Zhi Pu researchist of polytechnical university adopts polyvinyl alcohol hydration solvent to improve the mechanical property of YBCO presoma blank as binding agent, thereby suppress the formation of crackle in superconductive block process of growth, research is found that the interpolation of binding agent has obviously reduced and is oozed the crackle in superconductive block after oxygen, but do not affect its superconductivity.Thereby Tomita and the Murakami etc. in Japan's superconductor technology research centre propose the mechanical property of the expansion raising superconductive block that adopts resin injection technology to stop crackle, they also study and find that interpolation Ag can improve the mechanical property of superconductive block, this technology is greatly improved the mechanical property of YBCO and improves, but find that silver-colored interpolation can reduce the growth velocity of YBCO bulk, unfavorable to preparation large size superconductive block.
Result of study discovery, metallic oxide crystal whisker material can significantly strengthen the performance of body material.But up to now, in the preparation process of YBCO bulk, introduce metallic oxide crystal whisker as reinforcement, the correlative study that obtains high mechanical strength YBCO superconducting material has no report.
Summary of the invention
Technical problem to be solved by this invention is for above-mentioned the deficiencies in the prior art, and a kind of preparation method of YBCO superconductive block of metallic oxide crystal whisker enhancing is provided.The method preparation technology's simple possible, has the features such as efficient, easy control of reaction system, is suitable for large-scale industrial production; The magnetic suspension force of the YBCO superconductive block that metallic oxide crystal whisker prepared by employing the method strengthens is high, and superconductivity and mechanical property are good.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the preparation method of the YBCO superconductive block that a kind of metallic oxide crystal whisker strengthens, it is characterized in that, and the method comprises the following steps:
Step 1, prepare the first powder mix and the second powder mix respectively:
Step 101, add in mortar ground and mixed even Y123 powder, Y211 powder and metallic oxide crystal whisker, obtain the first powder mix; In described the first powder mix, the quality percentage composition of metallic oxide crystal whisker is 5%～15%, and in described the first powder mix, the mol ratio of Y123 powder and Y211 powder is 1: 0.3;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix;
Step 2, prepare powder compact:
Step 201, the first powder mix described in step 101 is added in compacting tool set, then utilize oil press to carry out precompressed processing to the first powder mix in compacting tool set; The pressure of described precompressed processing is 5MPa～6MPa;
Step 202, the second powder mix described in step 102 is added in compacting tool set and be layed in the top of precompressed the first powder mix after treatment, then utilize oil press to the first powder mix in compacting tool set and the second powder mix compression moulding, after the demoulding, obtain powder compact; The pressure of described compression moulding is 10MPa～20MPa; In described powder compact, the quality percentage composition of the second powder mix is 10%～15%, and surplus is the first powder mix;
Step 3, seed crystal is positioned over to the top of powder compact described in step 202, then, under air atmosphere, the powder compact that utilizes tube furnace to be placed with seed crystal to top carries out crystallization processing, obtains single domain bulk;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, after furnace cooling, obtain metallic oxide crystal whisker strengthen YBCO superconductive block.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, is characterized in that, metallic oxide crystal whisker described in step 101 is Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, is characterized in that, the length-to-diameter ratio of metallic oxide crystal whisker described in step 101 is not less than 20.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, is characterized in that, metallic oxide crystal whisker described in step 101 is nanosize metal oxide whisker or micron order metallic oxide crystal whisker.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, is characterized in that, seed crystal described in step 3 is NdBaCuO seed crystal.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, it is characterized in that, the concrete system of the processing of crystallization described in step 3 is: the powder compact that top is placed with to seed crystal is incubated 2h after being warming up to 1040 DEG C～1055 DEG C with the temperature rise rate of 100 DEG C/h～120 DEG C/h, be cooled to 1000 DEG C～1010 DEG C with the rate of temperature fall of 70 DEG C/h～90 DEG C/h again, then be cooled to 970 DEG C～980 DEG C with the rate of temperature fall of 0.2 DEG C/h～0.5 DEG C/h, finally cool to 25 DEG C of room temperatures with the furnace.
The preparation method of the YBCO superconductive block that above-mentioned a kind of metallic oxide crystal whisker strengthens, is characterized in that, the temperature of oozing oxygen processing described in step 4 is 400 DEG C～500 DEG C, described in ooze oxygen processing time be 60h～100h.
The present invention compared with prior art has the following advantages:
1, the present invention adds metallic oxide crystal whisker as reinforcement in the preparation process of YBCO superconductive block, take full advantage of the characteristic of metallic oxide crystal whisker high strength, high-modulus and high elongation rate, the internal bond strength of YBCO bulk is been significantly enhanced, the single crystal fibre structure of metallic oxide crystal whisker can be used as pinning center simultaneously, can greatly improve the superconductivity of YBCO superconductive block.
2, the present invention studies discovery, and the adding procedure of metallic oxide crystal whisker has remarkably influenced for the superconductivity of made YBCO bulk.If by Y123 powder, Y211 powder and metallic oxide crystal whisker simply ground and mixed be pressed into base after evenly, in crystallization process, due to the existence of metallic oxide crystal whisker, the flux growth process to seed crystal exerts an influence in meeting, cause forming mixed and disorderly multidomain body, the magnetic suspension force of made YBCO bulk is low, and superconductivity is poor.Therefore, the present invention is by repeatedly adjusting and optimize processing parameter, final design goes out a set of efficient, feasible technical scheme, first by part Y123 powder, part Y211 powder and metallic oxide crystal whisker mixing precompressed, and then add a small amount of Y123 powder and the powder mix of Y211 powder in the above, thereby metallic oxide crystal whisker and seed crystal are effectively isolated to get up, in seed crystal infiltration crystallization process, eliminate the impact of metallic oxide crystal whisker completely and formed perfect single-domain body, the magnetic suspension force of final made YBCO bulk is high, and superconductivity is good.
The critical transition temperature of the YBCO superconductive block that the metallic oxide crystal whisker that 3, prepared by employing the present invention strengthens is 89K～90K, and breaking tenacity reaches 95MPa～105MPa, and magnetic suspension force density reaches 10N/cm 2～14N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present invention strengthens is described is thus high, and superconductivity and mechanical property are good.
4, the present invention is incorporated into the enhanced process of matrix material subject the preparation field of superconductive block, provides new thinking for preparing high performance superconductive block; Agent technology thought of the present invention can also expand to preparation and the production of the superconductive blocks such as GdBCO, SmBCO, NdBCO.
5, preparation method's simple possible of the present invention, has the features such as efficient, easy control of reaction system, is suitable for large-scale industrial production.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Brief description of the drawings
Fig. 1 is preparation technology's schema of the YBCO superconductive block of metallic oxide crystal whisker enhancing of the present invention.
Fig. 2 is the cross-sectional view that the compacting tool set of the first powder mix and the second powder mix is equipped with in the present invention.
Fig. 3 is the structural representation that top of the present invention is placed with the powder compact of seed crystal.
Description of reference numerals:
1-the first powder mix; 2-the second powder mix; 3-compacting tool set;
4-powder compact; 5-seed crystal.
Embodiment
Embodiment 1
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 5%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is that length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) is not less than 20 nano level Al 2o 3whisker;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 5MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 10MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 15%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1045 DEG C with the temperature rise rate of 120 DEG C/h, be incubated 2h, then be cooled to 1005 DEG C with the rate of temperature fall of 80 DEG C/h, be cooled to 980 DEG C with the rate of temperature fall of 0.5 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 450 DEG C, described in ooze oxygen processing time be 60h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 90K, and breaking tenacity is 96MPa, and magnetic suspension force density is 10N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 2
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 10%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is that length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) is not less than 20 micron order TiO 2whisker;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 6MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 20MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 15%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1040 DEG C with the temperature rise rate of 100 DEG C/h, be incubated 2h, then be cooled to 1000 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 970 DEG C with the rate of temperature fall of 0.2 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 500 DEG C, described in ooze oxygen processing time be 100h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 90K, and breaking tenacity is 99MPa, and magnetic suspension force density is 10.6N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 3
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 15%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is not less than 20 micron order Al by length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) 2o3 whisker and length-to-diameter ratio are not less than 20 micron order TiO 2whisker mixes in mass ratio at 2: 1;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 5MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 10MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 12%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1045 DEG C with the temperature rise rate of 110 DEG C/h, be incubated 2h, then be cooled to 1000 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 970 DEG C with the rate of temperature fall of 0.5 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 500 DEG C, described in ooze oxygen processing time be 100h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 89K, and breaking tenacity is 98MPa, and magnetic suspension force density is 12.6N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 4
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 15%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is not less than 20 micron order Al by length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) 2o3 whisker and length-to-diameter ratio are not less than 20 micron order TiO 2whisker mixes in mass ratio at 1: 3;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 6MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 20MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 10%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1055 DEG C with the temperature rise rate of 120 DEG C/h, be incubated 2h, then be cooled to 1010 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 980 DEG C with the rate of temperature fall of 0.2 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 500 DEG C, described in ooze oxygen processing time be 60h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 89.5K, and breaking tenacity is 105MPa, and magnetic suspension force density is 13.2N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 5
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 10%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is not less than 20 micron order Al by length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) 2o 3whisker and length-to-diameter ratio are not less than 20 micron order TiO 2whisker mixes in mass ratio at 1: 5;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 5.5MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 15MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 12%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1050 DEG C with the temperature rise rate of 110 DEG C/h, be incubated 2h, then be cooled to 1005 DEG C with the rate of temperature fall of 80 DEG C/h, be cooled to 975 DEG C with the rate of temperature fall of 0.3 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 450 DEG C, described in ooze oxygen processing time be 80h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 89.5K, and breaking tenacity is 102MPa, and magnetic suspension force density is 14N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 6
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 9%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is that length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) is not less than 20 micron order MgO whisker;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 6MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 20MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 15%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1040 DEG C with the temperature rise rate of 100 DEG C/h, be incubated 2h, then be cooled to 1000 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 970 DEG C with the rate of temperature fall of 0.2 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 450 DEG C, described in ooze oxygen processing time be 80h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 90K, and breaking tenacity is 99MPa, and magnetic suspension force density is 10.5N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 7
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 8%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is not less than 20 micron order Al by length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) 2o 3whisker, length-to-diameter ratio are not less than 20 micron order TiO 2whisker and length-to-diameter ratio are not less than 20 micron order MgO whisker and mix at 1: 2: 3 in mass ratio;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 5MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 18MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 15%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1040 DEG C with the temperature rise rate of 100 DEG C/h, be incubated 2h, then be cooled to 1000 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 970 DEG C with the rate of temperature fall of 0.2 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 480 DEG C, described in ooze oxygen processing time be 90h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 90K, and breaking tenacity is 100MPa, and magnetic suspension force density is 11.8N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
Embodiment 8
In conjunction with Fig. 1, Fig. 2 and Fig. 3, the preparation method of the YBCO superconductive block that the present embodiment metallic oxide crystal whisker strengthens comprises the following steps:
Step 1, prepare the first powder mix 1 and the second powder mix 2 respectively:
Step 101, be YBa by Y123(Y123 2cu 3o 7-x) powder, Y211(Y211 be Y 2baCuO 5) powder and metallic oxide crystal whisker add in mortar ground and mixed even, obtains the first powder mix 1; In described the first powder mix 1, the quality percentage composition of metallic oxide crystal whisker is 10%, and in described the first powder mix 1, the mol ratio of Y123 powder and Y211 powder is 1: 0.3; Described metallic oxide crystal whisker is preferably Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker, the metallic oxide crystal whisker that the present embodiment adopts is not less than 20 nano level Al by length-to-diameter ratio (length-to-diameter ratio refers to the length of metallic oxide crystal whisker and the ratio of diameter of section) 2o 3whisker, length-to-diameter ratio are not less than 20 nano level TiO 2whisker and length-to-diameter ratio are not less than 20 nano level MgO whisker and mix at 2: 3: 1 in mass ratio;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix 2;
Step 2, prepare powder compact 4:
Step 201, the first powder mix 1 described in step 101 is added in compacting tool set 3, then utilize oil press to carry out precompressed processing to the first powder mix 1 in compacting tool set 3; The pressure of described precompressed processing is 5MPa;
Step 202, the second powder mix 2 described in step 102 is added in compacting tool set 3 and be layed in the top of precompressed the first powder mix 1 after treatment, then utilize oil press to be pressed to the first powder mix 1 in compacting tool set 3 and the second powder mix 2, after the demoulding, obtain powder compact 4; The pressure of described compression moulding is 15MPa; In described powder compact 4, the quality percentage composition of the second powder mix 2 is 15%, and surplus is the first powder mix 1;
Step 3, seed crystal 5 is positioned over to the top of powder compact 4 described in step 202, then, under air atmosphere, the powder compact 4 that utilizes tube furnace to be placed with seed crystal 5 to top carries out crystallization processing, obtains single domain bulk; Described seed crystal 5 is NdBaCuO seed crystal; The concrete system of described crystallization processing is: after the powder compact 4 that first top is placed with to seed crystal 5 is warming up to 1040 DEG C with the temperature rise rate of 100 DEG C/h, be incubated 2h, then be cooled to 1000 DEG C with the rate of temperature fall of 70 DEG C/h, be cooled to 970 DEG C with the rate of temperature fall of 0.2 DEG C/h again, finally cool to 25 DEG C of room temperatures with the furnace;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, the temperature of oozing oxygen processing is 400 DEG C, described in ooze oxygen processing time be 60h, after furnace cooling, obtain the YBCO superconductive block that metallic oxide crystal whisker strengthens.
The critical transition temperature of the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is 90K, and breaking tenacity is 99.5MPa, and magnetic suspension force density is 12N/cm 2; The magnetic suspension force that the YBCO superconductive block that metallic oxide crystal whisker prepared by the present embodiment strengthens is described is high, and has good superconductivity and mechanical property.
The above, be only preferred embodiment of the present invention, not the present invention imposed any restrictions.Every any simple modification of above embodiment being done according to invention technical spirit, change and equivalence change, and all still belong in the protection domain of technical solution of the present invention.

Claims (4)

1. a preparation method for the YBCO superconductive block that metallic oxide crystal whisker strengthens, is characterized in that, the method comprises the following steps:
Step 1, prepare the first powder mix (1) and the second powder mix (2) respectively:
Step 101, add in mortar ground and mixed even Y123 powder, Y211 powder and metallic oxide crystal whisker, obtain the first powder mix (1); In described the first powder mix (1), the quality percentage composition of metallic oxide crystal whisker is 5%～15%, and in described the first powder mix (1), the mol ratio of Y123 powder and Y211 powder is 1: 0.3;
Step 102, within 1: 0.3 in molar ratio, add in mortar ground and mixed even in Y123 powder and Y211 powder, obtain the second powder mix (2);
Step 2, prepare powder compact (4):
Step 201, the first powder mix described in step 101 (1) is added in compacting tool set (3), then utilize oil press to carry out precompressed processing to the first powder mix (1) in compacting tool set (3); The pressure of described precompressed processing is 5MPa～6MPa;
Step 202, the second powder mix described in step 102 (2) is added in compacting tool set (3) and be layed in the top of precompressed the first powder mix after treatment (1), then utilize oil press to the first powder mix (1) in compacting tool set (3) and the second powder mix (2) compression moulding, after the demoulding, obtain powder compact (4); The pressure of described compression moulding is 10MPa～20MPa; In described powder compact (4), the quality percentage composition of the second powder mix (2) is 10%～15%, and surplus is the first powder mix (1);
Step 3, seed crystal (5) is positioned over to the top of powder compact described in step 202 (4), then under air atmosphere, the powder compact (4) that utilizes tube furnace to be placed with seed crystal (5) to top carries out crystallization processing, obtains single domain bulk;
Step 4, under oxygen atmosphere, utilize tube furnace to ooze oxygen processing to the bulk of single domain described in step 3, after furnace cooling, obtain metallic oxide crystal whisker strengthen YBCO superconductive block;
Metallic oxide crystal whisker described in step 101 is Al 2o 3whisker, TiO 2one or more in whisker and MgO whisker;
The concrete system of the processing of crystallization described in step 3 is: the powder compact (4) that top is placed with to seed crystal (5) is incubated 2h after being warming up to 1040 DEG C～1055 DEG C with the temperature rise rate of 100 DEG C/h～120 DEG C/h, be cooled to 1000 DEG C～1010 DEG C with the rate of temperature fall of 70 DEG C/h～90 DEG C/h again, then be cooled to 970 DEG C～980 DEG C with the rate of temperature fall of 0.2 DEG C/h～0.5 DEG C/h, finally cool to 25 DEG C of room temperatures with the furnace;
The temperature of oozing oxygen processing described in step 4 is 400 DEG C～500 DEG C, described in ooze oxygen processing time be 60h～100h.
2. the preparation method of the YBCO superconductive block that a kind of metallic oxide crystal whisker according to claim 1 strengthens, is characterized in that, the length-to-diameter ratio of metallic oxide crystal whisker described in step 101 is not less than 20.
3. the preparation method of the YBCO superconductive block that a kind of metallic oxide crystal whisker according to claim 1 strengthens, is characterized in that, metallic oxide crystal whisker described in step 101 is nanosize metal oxide whisker or micron order metallic oxide crystal whisker.
4. the preparation method of the YBCO superconductive block that a kind of metallic oxide crystal whisker according to claim 1 strengthens, is characterized in that, seed crystal described in step 3 (5) is NdBaCuO seed crystal.
CN201310330195.1A 2013-07-31 2013-07-31 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers Active CN103360099B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310330195.1A CN103360099B (en) 2013-07-31 2013-07-31 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310330195.1A CN103360099B (en) 2013-07-31 2013-07-31 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers

Publications (2)

Publication Number Publication Date
CN103360099A CN103360099A (en) 2013-10-23
CN103360099B true CN103360099B (en) 2014-08-06

Family

ID=49362460

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310330195.1A Active CN103360099B (en) 2013-07-31 2013-07-31 Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers

Country Status (1)

Country Link
CN (1) CN103360099B (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1446947A (en) * 2003-01-16 2003-10-08 上海交通大学 Method for preparing superconducting block material with thick film being as seed crystal fustion texture
CN101037339A (en) * 2007-04-25 2007-09-19 上海大学 Preparation method of high magnetic suspension force quasi-single domain yttrium, barium, copper and oxygen block
CN101475394A (en) * 2009-01-23 2009-07-08 清华大学 Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing
CN102584250A (en) * 2012-02-08 2012-07-18 上海交通大学 Method for preparing REBa2Cu3Ox (REBCO) high-temperature superconducting block material
CN102924075A (en) * 2012-11-29 2013-02-13 陕西师范大学 Method for producing single domain yttrium barium copper oxide superconduction block

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6414146A (en) * 1987-07-06 1989-01-18 Oki Electric Ind Co Ltd Ceramic superconductor

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1446947A (en) * 2003-01-16 2003-10-08 上海交通大学 Method for preparing superconducting block material with thick film being as seed crystal fustion texture
CN101037339A (en) * 2007-04-25 2007-09-19 上海大学 Preparation method of high magnetic suspension force quasi-single domain yttrium, barium, copper and oxygen block
CN101475394A (en) * 2009-01-23 2009-07-08 清华大学 Method for preparing large size yttrium system block material by Ag2O adding YBCO solder brazing
CN102584250A (en) * 2012-02-08 2012-07-18 上海交通大学 Method for preparing REBa2Cu3Ox (REBCO) high-temperature superconducting block material
CN102924075A (en) * 2012-11-29 2013-02-13 陕西师范大学 Method for producing single domain yttrium barium copper oxide superconduction block

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JP昭64-14146A 1989.01.18

Also Published As

Publication number Publication date
CN103360099A (en) 2013-10-23

Similar Documents

Publication Publication Date Title
CN107059127B (en) A kind of method of bottom seed crystal infiltration growth method preparation single domain rare earth barium copper oxide superconducting ring
CN103979951A (en) Method for preparing single-domain yttrium barium copper oxide bulk superconductor by taking Y2BaCuO5 as base material
CN104725035A (en) Preparation method of nano composite ytrium barium copper oxide superconducting bulks
CN103614775B (en) The method of the accurate single crystal of a kind of embedded seeded growth REBCO
CN102515189B (en) Preparation method of magnesium diboride superconducting material
CN100558634C (en) Superconduction MgB 2The low-temperature fast powder sintering method of nano particle
CN101168442B (en) High-performance MgB2 superconducting material and preparation method thereof
CN1929044B (en) MgB2 superconductive material containing Si element and C element and its preparing method
CN103541011B (en) The method of the accurate single crystal of a kind of growing RE BCO high-temperature superconductor
CN101295563B (en) Production method of MgB2 block material doped with organic matter
CN104217817B (en) Preparation (Ba/Sr)1-xkxfe2as2superconducting wire or the method for band
CN103360099B (en) Preparation method for YBCO superconductive block material enhanced by metal oxide crystal whiskers
CN101319379A (en) Method for 45 degree rare earth barium copper oxygen thin film seed high speed growth superconducting block material
CN101224897A (en) Cu doped MgB2 superconductor and low-temperature rapid preparation method
CN103603043B (en) The method of the accurate single crystal of a kind of embedded seeded growth calcium analysis YBCO
CN103361710B (en) Improve the method for single domain yttrium barium copper oxide superconductor preparation efficiency
CN103060914B (en) Notch cuttype accelerates the method for slow cooling quick growing RE BCO high-temperature superconductor block
CN105133014A (en) Method for growing REBCO high-temperature superconducting quasi single crystals
CN101508571B (en) Method for producing carbon doped MgB2 cryogenic conductor by step-by-step sintering reaction
CN105177712B (en) A kind of method of growth REBCO high-temperature superconducting blocks
CN103014861B (en) The preparation method of Pagoda-shaped large size REBCO high-temperature superconductor block
CN101319380B (en) Method for rare earth 242 phase control component for growing superconducting block material
CN110828059A (en) Hectometer-grade 37-core MgB2Magnesium diffusion preparation method of superconducting wire
CN102992771A (en) Method for producing magnesium diboride-based superconducting block
JP4125272B2 (en) MgB2 particle-Al composite material

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant