CN103361517A - High-capacity hydrogen storage alloy electrode material and production method thereof - Google Patents
High-capacity hydrogen storage alloy electrode material and production method thereof Download PDFInfo
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Abstract
The invention discloses a high-capacity hydrogen storage alloy electrode material which comprises the following chemical components in percentage by weight of 42-45 percent of La, 29-35 percent of Nd, 2-5 percent of Ce and 8-11 percent of Pr. The high-capacity hydrogen storage alloy electrode material has a chemical formula of ML1-x-ySmxMgyNizAlwCouMnv, wherein x is more than 0 and less than 6.7, y is more than 0 and less than 0.4, z is more than 3 and less than 4, w is more than 0.03 and less than 0.15, u is more than 0.03 and less than 0.15, v is more than 0.03 and less than 0.15, z+w+u+v is more than 3.1 and less than 4.2, and ML is a lanthanum-rich mixed rare earth metal. The invention also discloses a production method of the high-capacity hydrogen storage alloy electrode material. The high-capacity hydrogen storage alloy electrode material related in the invention has the advantages that the discharge specific capacity is 20-30 percent higher than that of a conventional AB5 type hydrogen storage alloy, and a good high-rate discharge property is achieved.
Description
Technical field
The present invention relates to a kind of material technology, specifically, relate to a kind of high capacity hydrogen storage alloy electrode material and production method thereof.
Background technology
Lanthanon hydrogen storage alloy is used for nickel-hydrogen battery negative pole material and starts from the 1980s, and initial nickel-hydrogen battery negative pole material adopts AB
5Type hydrogen storage alloy, and showing good specific energy and cycle life in numerous secondary cells at that time.Yet along with the development of society and the progress of battery industry, with AB
5Type hydrogen storage alloy is that the nickel metal hydride battery of negative material can not satisfy people gradually to the requirement of battery specific energy.
Disclose a kind of store hydrogen alloy electrode material such as Chinese patent CN1075380A, had preferably cyclical stability, its specific discharge capacity is about 280mAh/g; Chinese patent CN1078268A discloses a kind of hydrogen-storage alloy for hydrogen electrode and capacity method thereof, and the alloy of preparing has antioxygen and water, and to poison performance good, the stable lanthanon hydrogen storage alloy that is easy to activate in alkaline medium, and its specific discharge capacity is about 270mAh/g.
Along with the further investigation to lanthanon hydrogen storage alloy, it is found that a kind of alloy with super large cell configuration, its chemical formulation is A
2B
7, such hydrogen storage alloy has higher specific discharge capacity as electrode materials, is a kind of very promising novel hydrogen storage material.In the research in the past, A
2B
7Rare earth element in the hydrogen storage alloy is mainly take neodymium (Nd) as main, and along with the development in market, the price of Nd element goes up day by day, and this is to A
2B
7The market of type hydrogen storage alloy is used and has been caused obstruction.
Summary of the invention
Technical problem solved by the invention provides a kind of high capacity hydrogen storage alloy electrode material, its specific discharge capacity and traditional AB
5Type hydrogen storage alloy is compared and is exceeded 20%～30%, and has preferably high-rate discharge ability.
Technical scheme is as follows:
A kind of high capacity hydrogen storage alloy electrode material, its chemical constitution comprises ML according to weight percent meter
1-x-ySm
xMg
yNi
zAl
wCo
uMn
v, 0＜x＜6.7,0＜y＜0.4,3＜z＜4,0.03＜w＜0.15,0.03＜u＜0.15,0.03＜v＜0.15 wherein, elementary composition pass is 3.1＜z+w+u+v＜4.2; ML is lanthanum rich norium, and composition is: La42%～45%, Nd29%～35%, Ce2%～5%, Pr8%～11%.
Further: its moiety is ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08
Further: its moiety is ML
0.57Sm
0.22Mg
0.21Ni
3.07Al
0.12Co
0.08Mn
0.2
Further: described high capacity hydrogen storage alloy electrode material is 300～400 purpose powdered alloys.
Another technical problem solved by the invention provides a kind of production method of high capacity hydrogen storage alloy electrode material, obtains the high capacity hydrogen storage alloy electrode material, its specific discharge capacity and traditional AB
5Type hydrogen storage alloy is compared and is exceeded 20%～30%, and has preferably high-rate discharge ability.
Technical scheme is as follows:
A kind of production method of high capacity hydrogen storage alloy electrode material, prepare the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace, comprise charging, fusing, refining, casting and annealing process, the chemical constitution of the high capacity hydrogen storage alloy electrode material that obtains comprises ML according to weight percent meter
1-x-ySm
xMg
yNi
zAl
wCo
uMn
v, 0＜x＜6.7,0＜y＜0.4,3＜z＜4,0.03＜w＜0.15,0.03＜u＜0.15,0.03＜v＜0.15 wherein, elementary composition pass is 3.1＜z+w+u+v＜4.2; ML is lanthanum rich norium, and composition is: La42%～45%, Nd29%～35%, Ce2%～5%, Pr8%～11%.
Further: preparing the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace, to obtain moiety be ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08
Further: in the described charging process, to form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium, metal Sm, metal Co, metal Ni, metal A l, and the weight percent of described lanthanum rich norium, metal Sm, metal Co, metal Ni, metal A l is followed successively by 11.2%, 27.6%, 1.4%, 58.5%, 0.5%;
In the described melting process, be evacuated to first before the melting below 1 * 10-2MPa, be filled with again an amount of argon gas and make vacuum keep at 0.06MPa; First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually;
In described refining and the casting cycle, continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06Mpa, refining 3 minutes, next reduce power, make temperature remain on 1000 ℃～1300 ℃, when melt liquid level has just begun to crust Mg is added by the secondary charging bucket; Then be warming up to 1400 ℃～1500 ℃, vacuum tightness 0.06Mpa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, and vacuum tightness 0.06MPa casts;
In the described annealing process, at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
Further: the moiety for preparing the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace is ML
0.57Sm
0.22Mg
0.21Ni
3.07Al
0.12Co
0.08Mn
0.2
Further: in the described charging process, to form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium, metal Sm, metal M n, metal Co, metal Ni, metal A l, and the weight percent of described lanthanum rich norium, metal Sm, metal M n, metal Co, metal Ni, metal A l is followed successively by 25.2%, 10.4%, 3.5%, 1.5%, 56.8%, 1.0%;
In the described melting process, be evacuated to first before the melting below 1 * 10-2MPa, be filled with again an amount of argon gas and make vacuum keep about 0.06MPa.First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually.
In described refining and the casting cycle, continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06MPa, refining 3 minutes, next reduce power, make temperature remain on 1000 ℃～1300 ℃, when melt liquid level has just begun to crust Mg is added by the secondary charging bucket; Then be warming up to rapidly 1400 ℃～1500 ℃, vacuum tightness 0.06MPa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, and vacuum tightness 0.06MPa casts;
In the described annealing process, at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
Further: the alloy pig that obtains is worn into 300～400 purpose powdered alloys with vibromill behind surface cleaning.
The present invention compared with prior art has the following advantages:
1, the high capacity hydrogen storage alloy electrode material that the present invention relates to, its specific discharge capacity and traditional AB
5Type hydrogen storage alloy is compared and is exceeded 20%～30%, and has preferably high-rate discharge ability.
2, the high capacity hydrogen storage alloy electrode material of the present invention's design, its material cost is low, and preparation technology and equipment are simple, and energy consumption is few, is easy to industrialization and popularization.
Embodiment
The object of the present invention is to provide a kind of relatively inexpensive Samarium Nitrate of employing (Sm) to substitute the A that Nd prepares
2B
7Type hydrogen storage alloy.The present invention can significantly reduce the material cost of this base hydrogen storage alloy, and the hydrogen storage alloy of preparation has good high-rate discharge ability and higher specific discharge capacity.
The invention provides a kind of high capacity hydrogen storage alloy electrode material, its chemical constitution comprises according to weight percent meter:
ML
1-x-ySm
xMg
yNi
zAl
wCo
uMn
v, 0＜x＜6.7 wherein; 0＜y＜0.4; 3＜z＜4; 0.03＜w＜0.15; 0.03＜u＜0.15; 0.03＜v＜0.15.Upper each elementary composition pass is 3.1＜z+w+u+v＜4.2.
ML is lanthanum rich norium, and composition is: La42%～45%, Nd29%～35%, Ce2%～5%, Pr8%～11%.
When preparing the high capacity hydrogen storage alloy electrode material of heterogeneity ratio with vacuum induction melting furnace, used parameter is identical, below by two embodiment the material preparation process is elaborated.
Embodiment 1
Preparing composition with vacuum induction melting furnace is ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08Alloy pig, the parameter of fusion process and employing is as follows:
Step 11: charging;
To form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium → metal Sm → metal Co → metal Ni → metal A l, the weight percent of lanthanum rich norium, metal Sm, metal Co, metal Ni, metal A l is followed successively by 11.2%, 27.6%, 1.4%, 58.5%, 0.5%.
Step 12: fusing;
Be evacuated to first 1 * 10 before the melting
-2Below the MPa, be filled with again an amount of argon gas and make vacuum keep about 0.06MPa.First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually.
Step 13: refining and casting;
Then continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06MPa, refining 3 minutes; next reduce power; make temperature remain on 1000 ℃～1300 ℃, melt liquid level has just begun crust is advisable, and Mg is added by the secondary charging bucket again.Then be warming up to rapidly 1400 ℃～1500 ℃, vacuum tightness 0.06MPa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, vacuum tightness 0.06MPa, and casting gets final product.
Step 14: annealing.
After the melting with it at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
To wear into 300～400 purpose powdered alloys with vibromill after the alloy surface purification.The results are shown in Table 1 for the electrochemistry capacitance that its test obtains.
Table 1ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08Alloy half-cell test result
| Discharge-rate | 1C | 2C | 3C |
| Loading capacity (mAh/g) | 348.8 | 312.5 | 302.3 |
Embodiment 2
Preparing composition with vacuum induction melting furnace is ML
0.57Sm
0.22Mg
0.21Ni
3.07Al
0.12Co
0.08Mn
0.2Alloy pig.The parameter of fusion process and employing is as follows:
Step 21: charging;
At first will form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium → metal Sm → metal M n → metal Co → metal Ni → metal A l, the weight percent of lanthanum rich norium, metal Sm, metal M n, metal Co, metal Ni, metal A l is followed successively by 25.2%, 10.4%, 3.5%, 1.5%, 56.8%, 1.0%.
Step 21: fusing;
Be evacuated to first 1 * 10 before the melting
-2Below the MPa, be filled with again an amount of argon gas and make vacuum keep about 0.06MPa.First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually.
Step 23: refining and casting;
Then continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06Mpa, refining 3 minutes; next reduce power; make temperature remain on 1000 ℃～1300 ℃, melt liquid level has just begun crust is advisable, and Mg is added by the secondary charging bucket again.Then be warming up to rapidly 1400 ℃～1500 ℃, vacuum tightness 0.06MPa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, vacuum tightness 0.06MPa, and casting gets final product.
Step 24: annealing.
After the melting with it at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
To wear into 300～400 purpose powdered alloys with vibromill behind its surface cleaning.The results are shown in Table 2 for the electrochemistry capacitance that its test obtains.
Table 2ML
057Sm
022Mg
021Ni
307Al
012Co
008Mn
02Alloy half-cell test result
| Discharge-rate | 1C | 2C | 3C |
| Loading capacity (mAh/g) | 357.5 | 303.5 | 287.5 |
Claims (10)
1. high capacity hydrogen storage alloy electrode material, it is characterized in that: its chemical constitution comprises ML according to weight percent meter
1-x-ySm
xMg
yNi
zAl
wCo
uMn
v, 0＜x＜6.7,0＜y＜0.4,3＜z＜4,0.03＜w＜0.15,0.03＜u＜0.15,0.03＜v＜0.15 wherein, elementary composition pass is 3.1＜z+w+u+v＜4.2; ML is lanthanum rich norium, and composition is: La42%～45%, Nd29%～35%, Ce2%～5%, Pr8%～11%.
2. high capacity hydrogen storage alloy electrode material as claimed in claim 1, it is characterized in that: its moiety is ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08
3. high capacity hydrogen storage alloy electrode material as claimed in claim 1, it is characterized in that: its moiety is ML
0.57Sm
0.22Mg
0.21Ni
3.07Al
0.12Co
0.08Mn
0.2
4. such as claims 1 to 3 high capacity hydrogen storage alloy electrode material as described in each, it is characterized in that: described high capacity hydrogen storage alloy electrode material is 300～400 purpose powdered alloys.
5. the production method of a high capacity hydrogen storage alloy electrode material, prepare the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace, comprise charging, fusing, refining, casting and annealing process, it is characterized in that: the chemical constitution of the high capacity hydrogen storage alloy electrode material that obtains comprises ML according to weight percent meter
1-x-ySm
xMg
yNi
zAl
wCo
uMn
v, 0＜x＜6.7,0＜y＜0.4,3＜z＜4,0.03＜w＜0.15,0.03＜u＜0.15,0.03＜v＜0.15 wherein, elementary composition pass is 3.1＜z+w+u+v＜4.2; ML is lanthanum rich norium, and composition is: La42%～45%, Nd29%～35%, Ce2%～5%, Pr8%～11%.
6. the production method of high capacity hydrogen storage alloy electrode material as claimed in claim 5 is characterized in that: preparing the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace, to obtain moiety be ML
0.27Sm
0.62Mg
0.11Ni
3.37Al
0.06Co
0.08
7. the production method of high capacity hydrogen storage alloy electrode material as claimed in claim 6 is characterized in that:
In the described charging process, to form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium, metal Sm, metal Co, metal Ni, metal A l, and the weight percent of described lanthanum rich norium, metal Sm, metal Co, metal Ni, metal A l is followed successively by 11.2%, 27.6%, 1.4%, 58.5%, 0.5%;
In the described melting process, be evacuated to first 1 * 10 before the melting
-2Below the MPa, be filled with again an amount of argon gas and make vacuum keep at 0.06MPa; First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually;
In described refining and the casting cycle, continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06Mpa, refining 3 minutes, next reduce power, make temperature remain on 1000 ℃～1300 ℃, when melt liquid level has just begun to crust Mg is added by the secondary charging bucket; Then be warming up to 1400 ℃～1500 ℃, vacuum tightness 0.06Mpa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, and vacuum tightness 0.06Mpa casts;
In the described annealing process, at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
8. the production method of high capacity hydrogen storage alloy electrode material as claimed in claim 5, it is characterized in that: the moiety for preparing the high capacity hydrogen storage alloy electrode material with vacuum induction melting furnace is ML
0.57Sm
0.22Mg
0.21Ni
3.07Al
0.12Co
0.08Mn
0.2
9. the production method of high capacity hydrogen storage alloy electrode material as claimed in claim 8 is characterized in that:
In the described charging process, to form the raw material weigh up by design packs in the smelting pot of vacuum induction melting furnace, order of addition(of ingredients) is: lanthanum rich norium, metal Sm, metal M n, metal Co, metal Ni, metal A l, and the weight percent of described lanthanum rich norium, metal Sm, metal M n, metal Co, metal Ni, metal A l is followed successively by 25.2%, 10.4%, 3.5%, 1.5%, 56.8%, 1.0%;
In the described melting process, be evacuated to first 1 * 10 before the melting
-2Below the MPa, be filled with again an amount of argon gas and make vacuum keep about 0.06MPa.First progressively be warmed up to 1200 ℃～1350 ℃ during melting, kept power 3 minutes, raw material is melted gradually.
In described refining and the casting cycle, continue to be warming up to 1400 ℃～1500 ℃, the vacuum degree control under the argon shield is at 0.06Mpa, refining 3 minutes, next reduce power, make temperature remain on 1000 ℃～1300 ℃, when melt liquid level has just begun to crust Mg is added by the secondary charging bucket; Then be warming up to rapidly 1400 ℃～1500 ℃, vacuum tightness 0.06Mpa kept 1～2 minute, reduced at last temperature to 1300 ℃～1400 ℃, and vacuum tightness 0.06Mpa casts;
In the described annealing process, at 800～1300 ℃, the thermal treatment 10～20h that anneals under the 0.5atm ar gas environment obtains the alloy of homogeneous chemical composition.
10. such as the production method of claim 5 to 9 high capacity hydrogen storage alloy electrode material as described in each, it is characterized in that: the alloy pig that obtains is worn into 300～400 purpose powdered alloys with vibromill behind surface cleaning.
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| CN108199009A (en) * | 2017-12-29 | 2018-06-22 | 东莞市朗泰通实业有限公司 | A kind of low-temperature nickel-hydrogen battery of cathode coated on both sides |
| CN108893656A (en) * | 2018-05-30 | 2018-11-27 | 安泰科技股份有限公司 | La-Mg-Ni system A2B7Type hydrogen storage alloy and preparation method thereof |
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