CN108847486A - A kind of preparation method of the nickel phosphide microballoon of multilevel structure - Google Patents
A kind of preparation method of the nickel phosphide microballoon of multilevel structure Download PDFInfo
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- CN108847486A CN108847486A CN201810598701.8A CN201810598701A CN108847486A CN 108847486 A CN108847486 A CN 108847486A CN 201810598701 A CN201810598701 A CN 201810598701A CN 108847486 A CN108847486 A CN 108847486A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5805—Phosphides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
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- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- Y02E60/10—Energy storage using batteries
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Abstract
A kind of preparation method of the nickel phosphide microballoon of multilevel structure, the present invention relates to the preparation methods of nickel phosphide.The present invention is to solve the low technical problems of existing nickel phosphide tap density.This method：One, presoma is prepared with nickel acetate and urea；Two, presoma is put into a porcelain boat; sodium hypophosphite is put into another porcelain boat again; two porcelain boats are put into quartz ampoule together; argon gas protection is continually fed into quartz ampoule; the porcelain boat for wherein filling sodium hypophosphite is put into the upstream of air-flow; then quartz ampoule is warming up to 300~400 DEG C and keeps the temperature 4~6 hours, obtain the nickel phosphide microballoon of multilevel structure.Nickel phosphide microballoon of the invention is made of the phosphatization nickel nano film of secondary structure, the specific surface area of nickel phosphide microballoon can be improved using the multilevel structure of nickel phosphide microballoon, increase the contact area with electrolyte, and tap density is high, there is higher volume and capacity ratio.Preparation method is simple, mild condition.It can be used for making negative electrode of lithium ion battery.
Description
Technical field
The present invention relates to the preparation methods of nickel phosphide.
Background technique
With the development of society, the demand to energy storage device is higher and higher, and the utilization of reversible lithium ion battery is also more next
It is more extensive.Electrode material is component part important in lithium ion battery, and developing has height ratio capacity, quick charge and discharge
Electric, long circulating stability new electrode materials are of great significance.There are many transition metal oxide is high due to having now
Specific capacity and be applied to lithium ion battery, but the electron conduction of transition metal oxide is poor, so that transition metal oxide
Poor charge-discharge magnification performance.And transition metal phosphide has lower charge and discharge potential, higher electron conduction, one
Fixed metalline, preferable thermal stability, higher specific capacity and the negative electrode material for being used for lithium ion battery, but transition is golden
The volume of category phosphide volume change in charge and discharge process is bigger, causes capacity attenuation than more serious, in charge and discharge process
In cannot keep original specific capacity well.The electrode material of nano-scale has higher during lithium ion is embedded in
Invertibity, abundant compared with electrolyte contacts, the volume change of material is smaller；And nickel phosphide has low intercalation potential, it is high
Specific capacity and be applied to lithium ion battery negative material, the nickel phosphide for preparing nano-scale can improve nickel phosphide to a certain extent
The invertibity of electrode material.As the Chinese patent of Publication No. CN106495114A discloses a kind of preparation side of nano nickel phosphide
Method, this method, which uses six hydration nickel sulfate and yellow phosphorus and adds dipotassium hydrogen phosphate progress Liquid reduction reaction process, prepares nano nickel phosphide
Colloidal sol；Again using microwave heating reaction, after centrifugation, ethanol washing, drying up to nano nickel phosphide.This partial size is less than 10nm
Nano nickel phosphide due to the tap density of nano material it is not high.Existing phosphatization nickel particle exist again specific surface area it is small lack
It falls into, both materials volume and capacity ratio when being used as lithium ion battery negative material is lower.
Summary of the invention
The present invention is to solve the skills that existing nanoscale nickel phosphide tap density is low and nickel phosphide specific grain surface product is small
Art problem, and provide a kind of preparation method of the nickel phosphide microballoon of multilevel structure.
The preparation method of the nickel phosphide microballoon of multilevel structure of the invention, carries out according to the following steps：
One, presoma is prepared：
It is 1 by the molar ratio of nickel acetate and urea：(5~8), nickel acetate and urea are added to the water, and stirring and dissolving obtains
To mixed solution；Mixed solution is placed in the water-bath that temperature is 80~90 DEG C again and is kept for 3~5 hours, after cooling, is collected by centrifugation
Solid formation, then washes clean, then be dried in vacuo under conditions of temperature is 60~80 DEG C, obtain presoma；
Two, the nickel phosphide microballoon of multilevel structure is prepared：
The presoma that step 1 is obtained is put into a porcelain boat, then sodium hypophosphite is put into another porcelain boat, by two porcelain
Boat is put into quartz ampoule together, argon gas protection is continually fed into quartz ampoule, wherein the porcelain boat for filling sodium hypophosphite is put into air-flow
Upstream, then by quartz ampoule with the speed of 2~4 DEG C/min be warming up to 300~400 DEG C keep the temperature 4~6 hours, obtain multistage knot
The nickel phosphide microballoon of structure.
The present invention generates the nickel phosphide presoma microballoon of multilevel structure using nickel acetate, urea liquid water-bath, then leads to
Cross the nickel phosphide microballoon that the method for low temperature phosphor prepares the multilevel structure of black.Nickel phosphide microballoon of the invention is by secondary structure
Phosphatization nickel nano film composition, the specific surface area of nickel phosphide microballoon can be improved using the multilevel structure of nickel phosphide microballoon, increase
Add the contact area with electrolyte, the specific surface area of the nickel phosphide microballoon of multilevel structure prepared by the present invention is 12~14m2/ g,
Tap density is high simultaneously, has higher volume and capacity ratio.Preparation method is simple, mild condition.It can be used for making lithium-ion electric
Pond cathode.
Detailed description of the invention
Fig. 1 is to test the 1 multistage nickel phosphide microballoon XRD diffraction pattern being prepared；
Fig. 2 is to test the 1 nickel phosphide presoma SEM figure being prepared；
Fig. 3 is to test the 1 multistage nickel phosphide microballoon SEM figure being prepared；
Fig. 4 is to test the 2 multistage nickel phosphide microballoon SEM figures being prepared.
Specific embodiment
Specific embodiment one：The preparation method of the nickel phosphide microballoon of the multilevel structure of present embodiment, according to the following steps
It carries out：
One, presoma is prepared：
It is 1 by the molar ratio of nickel acetate and urea：(5~8), nickel acetate and urea are added to the water, and stirring and dissolving obtains
To mixed solution；Mixed solution is placed in the water-bath that temperature is 80~90 DEG C again and is kept for 3~5 hours, after cooling, is collected by centrifugation
Solid formation, then washes clean, then be dried in vacuo under conditions of temperature is 60~80 DEG C, obtain presoma；
Two, the nickel phosphide microballoon of multilevel structure is prepared：
The presoma that step 1 is obtained is put into a porcelain boat, then sodium hypophosphite is put into another porcelain boat, by two porcelain
Boat is put into quartz ampoule together, argon gas protection is continually fed into quartz ampoule, wherein the porcelain boat for filling sodium hypophosphite is put into air-flow
Upstream, then by quartz ampoule with the speed of 2~4 DEG C/min be warming up to 300~400 DEG C keep the temperature 4~6 hours, obtain multistage knot
The nickel phosphide microballoon of structure.
Specific embodiment two：The present embodiment is different from the first embodiment in that nickel acetate and urea in step 1
Molar ratio be 1：(6~7).It is other same as the specific embodiment one.
Specific embodiment three：The present embodiment is different from the first and the second embodiment in that mixed solution in step 1
The concentration of middle nickel acetate is 4~5g/L, and the concentration of urea is 7~9g/L.It is other the same as one or two specific embodiments.
Specific embodiment four：Water-bath in step 1 unlike one of present embodiment and specific embodiment one to three
Temperature is 70 DEG C, and water bath time is 4 hours.It is other identical as one of specific embodiment one to three.
Specific embodiment five：By stone in step 2 unlike one of present embodiment and specific embodiment one to four
English pipe is warming up to 350 DEG C with the speed of 3 DEG C/min and keeps the temperature 5 hours.It is other identical as one of specific embodiment one to four.
With verification experimental verification beneficial effects of the present invention below：
Test 1：The preparation method of the nickel phosphide microballoon of the multilevel structure of this test, carries out according to the following steps：
One, presoma is prepared：
98mg nickel acetate tetrahydrate and 160mg urea are added in the beaker for filling 20mL water, dissolution is stirred
30min obtains uniform mixed solution；Beaker is put into again, 3 hours are persistently stirred and kept the temperature in 90 DEG C of water-bath；System is cooling
To room temperature, solid formation is collected by centrifugation, then is washed with deionized water 3 times, with ethanol washing 2 times, is placed on the condition that temperature is 80 DEG C
Lower vacuum drying, obtains presoma；
Two, 100 milligrams of presoma for obtaining step 1 is put into a porcelain boat, then 1 gram of sodium hypophosphite is put into separately
In one porcelain boat, two porcelain boats are put into quartz ampoule together, argon gas protection are continually fed into quartz ampoule, wherein filling sodium hypophosphite
Porcelain boat be put into the upstream of air-flow, quartz ampoule is then warming up to 300 DEG C with the speed of 2 DEG C/min and keeps the temperature 4 hours, obtains black
Multilevel structure nickel phosphide microballoon.
The XRD diffraction spectrogram of the nickel phosphide microballoon of the multilevel structure for the black that this test procedure two obtains as shown in Figure 1, its
Middle a is the XRD diffraction spectrogram of the nickel phosphide microballoon for the multilevel structure that this test obtains, b Ni2The standard spectrogram of P.It can from Fig. 1
To find out, the nickel phosphide microballoon of the multilevel structure of this test synthesis is Ni2P。
The stereoscan photograph for the presoma that this test procedure one obtains is as shown in Fig. 2, figure it is seen that presoma
For multilevel structure microballoon.
The stereoscan photograph of the nickel phosphide microballoon of the multilevel structure for the black that this test procedure two obtains as shown in figure 3,
From figure 3, it can be seen that the diameter of nickel phosphide microballoon is about micron, microballoon is made of the phosphatization nickel nano film of secondary structure, is passed through
Test, the specific surface area of the nickel phosphide microballoon of the multilevel structure are 12m2/g。
Test 2：The preparation method of the nickel phosphide microballoon of the multilevel structure of this test, carries out according to the following steps：
One, presoma is prepared：
98mg nickel acetate tetrahydrate and 160mg urea are added in the beaker for filling 20mL water, dissolution is stirred
30min obtains uniform mixed solution；Beaker is put into again, 4 hours are persistently stirred and kept the temperature in 80 DEG C of water-bath；System is cooling
To room temperature, solid formation is collected by centrifugation, then is washed with deionized water 3 times, with ethanol washing 2 times, is placed on the condition that temperature is 80 DEG C
Lower vacuum drying, obtains presoma；
Two, 100 milligrams of presoma for obtaining step 1 is put into a porcelain boat, then 1 gram of sodium hypophosphite is put into separately
In one porcelain boat, two porcelain boats are put into quartz ampoule together, argon gas protection are continually fed into quartz ampoule, wherein filling sodium hypophosphite
Porcelain boat be put into the upstream of air-flow, quartz ampoule is then warming up to 400 DEG C with the speed of 2 DEG C/min and keeps the temperature 6 hours, obtains black
Multilevel structure nickel phosphide microballoon.
The nickel phosphide microballoon of the multilevel structure for the black that this test procedure two obtains is Ni2P.Its stereoscan photograph is as schemed
Shown in 4, from fig. 4, it can be seen that the diameter of nickel phosphide microballoon is about micron, microballoon by secondary structure phosphatization nickel nano film group
At after tested, the specific surface area of the nickel phosphide microballoon of the multilevel structure is 12.5m2/g。
Claims (5)
1. a kind of preparation method of the nickel phosphide microballoon of multilevel structure, it is characterised in that this method carries out according to the following steps：
One, presoma is prepared：
It is 1 by the molar ratio of nickel acetate and urea：(5~8), nickel acetate and urea are added to the water, and stirring and dissolving is mixed
Close solution；Mixed solution is placed in the water-bath that temperature is 80~90 DEG C again and is kept for 3~5 hours, after cooling, solid phase is collected by centrifugation
Object, then washes clean, then be dried in vacuo under conditions of temperature is 60~80 DEG C, obtain presoma；
Two, the nickel phosphide microballoon of multilevel structure is prepared：
The presoma that step 1 is obtained is put into a porcelain boat, then sodium hypophosphite is put into another porcelain boat, by two porcelain boats one
It rises and is put into quartz ampoule, argon gas protection is continually fed into quartz ampoule, wherein the porcelain boat for filling sodium hypophosphite is put into the upper of air-flow
Then quartz ampoule is warming up to 300~400 DEG C with the speed of 2~4 DEG C/min and keeps the temperature 4~6 hours, obtains multilevel structure by trip
Nickel phosphide microballoon.
2. a kind of preparation method of the nickel phosphide microballoon of multilevel structure according to claim 1, it is characterised in that step 1
The molar ratio of middle nickel acetate and urea is 1：(6~7).
3. a kind of preparation method of the nickel phosphide microballoon of multilevel structure according to claim 1 or 2, it is characterised in that step
The concentration of nickel acetate is 4~5g/L in mixed solution in one.
4. a kind of preparation method of the nickel phosphide microballoon of multilevel structure according to claim 1 or 2, it is characterised in that step
Bath temperature is 70 DEG C in one, and water bath time is 4 hours.
5. a kind of preparation method of the nickel phosphide microballoon of multilevel structure according to claim 1 or 2, it is characterised in that step
Quartz ampoule is warming up to 350 DEG C with the speed of 3 DEG C/min in two and keeps the temperature 5 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110518254A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of lithium metal battery negative current collector and its preparation method and application |
| CN112607716A (en) * | 2020-11-30 | 2021-04-06 | 天津大学 | Preparation method of nickel phosphide nanosheet and nickel phosphide nanosheet prepared by same |
| CN114195108A (en) * | 2022-01-05 | 2022-03-18 | 东北大学 | Magnetic field induced synthesis of Ni2P one-dimensional nano chain and preparation method and application thereof |
| CN114950506A (en) * | 2022-06-28 | 2022-08-30 | 南京信息工程大学 | Ni 2 P/ZnIn 2 S 4 Preparation method and application of heterojunction photocatalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107142488A (en) * | 2017-04-28 | 2017-09-08 | 南开大学 | A kind of porous multiple casing nickel phosphide tiny balloon and its preparation method and application |
| CN107376961A (en) * | 2017-07-25 | 2017-11-24 | 江苏大学 | Preparation and application of the integrated CoP nano-chip arrays as monoblock type class peroxidase |
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2018
- 2018-06-12 CN CN201810598701.8A patent/CN108847486A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107142488A (en) * | 2017-04-28 | 2017-09-08 | 南开大学 | A kind of porous multiple casing nickel phosphide tiny balloon and its preparation method and application |
| CN107376961A (en) * | 2017-07-25 | 2017-11-24 | 江苏大学 | Preparation and application of the integrated CoP nano-chip arrays as monoblock type class peroxidase |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110518254A (en) * | 2019-09-09 | 2019-11-29 | 厦门大学 | A kind of lithium metal battery negative current collector and its preparation method and application |
| CN112607716A (en) * | 2020-11-30 | 2021-04-06 | 天津大学 | Preparation method of nickel phosphide nanosheet and nickel phosphide nanosheet prepared by same |
| CN112607716B (en) * | 2020-11-30 | 2022-08-12 | 天津大学 | Preparation method of nickel phosphide nanosheet and nickel phosphide nanosheet prepared by same |
| CN114195108A (en) * | 2022-01-05 | 2022-03-18 | 东北大学 | Magnetic field induced synthesis of Ni2P one-dimensional nano chain and preparation method and application thereof |
| CN114950506A (en) * | 2022-06-28 | 2022-08-30 | 南京信息工程大学 | Ni 2 P/ZnIn 2 S 4 Preparation method and application of heterojunction photocatalyst |
| CN114950506B (en) * | 2022-06-28 | 2023-09-19 | 南京信息工程大学 | Ni (nickel) 2 P/ZnIn 2 S 4 Heterojunction photocatalyst preparation method and application thereof |
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Application publication date: 20181120 |