CN109560277A - A kind of preparation method of nanometer of linear manganese selenide/carbon composite - Google Patents
A kind of preparation method of nanometer of linear manganese selenide/carbon composite Download PDFInfo
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Abstract
A kind of nanometer of linear manganese selenide/carbon composite preparation method is with Mn (CH3COO)2·4H2O, the mixed solution of PVP-K30, ethyl alcohol and water, trimesic acid, selenium powder be raw material, respectively pass through nanometer threadiness metal organic framework compound Mn-BTC preparation, based on template construct the preparation of nanometer threadiness manganese selenide/carbon composite and etc. be made；Wherein, the mixed solution of the ethyl alcohol and water is to be obtained by mixing by volume for 1:1.Nano wire of the present invention is not easy to break, and pattern is uniform, good dispersion, is not in agglomeration, and manganese selenide/carbon composite purity is high, purity may be up to 99.1%, and yield is high, and up to 70% or more, storage capacity is big, has extended cycle life, in 100mA g‑1Current density under after 60 charge and discharge cycles, discharge capacity be 846.59mAh g‑1, storage capacity is big, and cycle-index at least can achieve 60 times, at most can up to 200 times, it is not in the suddenly big or suddenly small situation of electric current that use process stability is good, and process flow simple possible is worth marketing.
Description
Technical field
The invention belongs to new material technology fields, and in particular to one kind based on MOFs template construct nanometer threadiness manganese selenide/
The preparation method of carbon composite.
Background technique
With using petroleum as environmental pollution brought by the burning of the increasingly depleted and fossil energy of the fossil energy of representative
It gets worse, there is an urgent need to a kind of sustainable reproducible clean energy resourcies by people.And lithium ion battery is close with high-energy because of it
The advantages that degree, long circulation life, environment friendly, shows one's talent from numerous new energy, in mobile electronic device, new energy vapour
The fields such as vehicle have a wide range of applications.However, the negative electrode material of commercial Li-ion battery is graphite at present, the theoretical of graphite holds
Amount is only 372mAh/g, is unable to satisfy the capacity requirement of the large scale electronic equipments such as electric car, limits answering for lithium ion battery
With and development.Therefore scientist has developed capacity of a variety of negative electrode materials to improve lithium ion battery, such as Carbon Materials, transition
Metal oxide, transition metal sulfide, transition metal selenides etc..
Compared to transition metal oxide and transient metal sulfide, transition metal selenides not only has high volume ratio
Capacity and specific discharge capacity, and voltage platform is low polarize small, have preferable electric conductivity, be a kind of more potential lithium from
Sub- cell negative electrode material.However, similar with transition metal oxide, transition metal selenides is in charge and discharge process, due to lithium
The insertion and abjection of ion, it may occur that huge volume change leads to active material and collection to make active material breaking and Dusting
Fluid is detached from, and loses electrical contact, and capacity attenuation and cycle performance is caused to reduce.In addition, the electronic conduction of transition metal phosphide
Property is poor, hinders fast transfer of the electronics inside active material, limits its electrochemical response, leads to its fast charging and discharging
Ability and high rate performance are poor.
Currently, the research for improving transition metal selenides storage lithium performance is concentrated mainly on two aspects, one is by transition
The Carbon Materials such as metal selenide and graphene, carbon nanotube carry out it is compound, using the electric conductivity and mechanical performance that Carbon Materials are excellent,
Improve the electric conductivity of transition metal selenides and absorption cycle in the process because of stress caused by volume expansion；Another kind is to prepare
Transition metal selenides with nanoscale and porous structure expands the specific surface area of material, increases electrode material and electrolysis
The contact area of liquid shortens the diffusion path of electronics and lithium ion, and buffer volumes expand generated stress.
Metal organic framework compound, abbreviation MOFs are to pass through coordinate bond self assembly shape by organic ligand and metal ion
At the hybrid inorganic-organic materials with molecule hole.MOFs has porosity, bigger serface, component adjustability etc. excellent
Point, before making it that there is wide application in fields such as gas collection storage, gas separation, catalysis, sensor and energy storages
Scape has just had received widespread attention since last century the nineties are born.Simultaneously as the porous structure of MOFs and organic bone
The abundant adjustability of frame and metal ion makes it can be used as presoma to prepare porous material, such as Carbon Materials, metal oxygen
Compound, metal sulfide, metal selenide etc..Porous material derived from MOFs can retain porous structure possessed by MOFs and
Bigger serface, meanwhile, organic backbone can be changed into porous carbon under high temperature inert atmosphere, in the condition for not introducing external carbon source
Under can be prepared by porous carbon/metallic compound composite material.
Nanometer threadiness manganese selenide made from present/there are nano wires to be easily broken off for carbon composite, pattern is uneven, dispersion
Property it is poor, be easy to appear reunion, manganese selenide/carbon composite purity is not high, low yield, and storage capacity is small, and cycle life is short, use
Process stability is bad, is easy to appear the technical problems urgent need to resolve such as the suddenly big or suddenly small situation of electric current.
Summary of the invention
The preparation of nanometer threadiness manganese selenide/carbon composite is constructed based on MOFs template it is an object of that present invention to provide a kind of
Method.
The object of the invention is achieved through the following technical solutions:
The preparation method of a kind of nanometer of linear manganese selenide/carbon composite, which is characterized in that it is with Mn (CH3COO)2·
4H2O, the mixed solution of PVP-K30, ethyl alcohol and water, trimesic acid, selenium powder are raw material, pass through nanometer metallic threadlike respectively
The preparation of organic framework compounds Mn-BTC constructs nanometer threadiness manganese selenide/carbon composite preparation based on template；
Wherein, the mixed solution of the ethyl alcohol and water is to be obtained by mixing by volume for 1:1.
Further, the preparation of above-mentioned nanometer threadiness metal organic framework compound Mn-BTC is to take Mn (CH3COO)2·4H2O
It is dissolved in PVP-K30 in the mixed solution of ethyl alcohol and deionized water composition and 300 ~ 400 turns/min of revolving speed is set, mixing time is
6 ~ 10min dissolves to obtain mixed solution A；Trimesic acid is separately taken to be dissolved in the mixed solution of ethyl alcohol and deionized water composition, if
300 ~ 400 turns/min of revolving speed is set, mixing time is 6 ~ 10min, dissolves to obtain solution B；Then solution A is added dropwise under agitation
Enter in solution B, stir 10min ~ 20min, stop stirring, place aging 20 ~ for 24 hours at room temperature, product is then centrifuged 15000
Turn/min, collect centrifugation, then washs precipitating 3 times with the mixed solution of ethyl alcohol and deionized water, the precipitating and ethyl alcohol
It is 1:100 ~ 1:150 with the mixed liquor volume ratio of deionized water, precipitating is placed in 55 ~ 65 DEG C of air dryings, dry 12 ~
15h, products therefrom are nanometer threadiness metal organic framework compound Mn-BTC, and white is presented in product, and shape is that nanometer is linear.
Further, above-mentioned Mn (CH3COO)2·4H2The mass ratio of O and PVP-K30 is 0.2449 ~ 0.4898:1 ~ 3, unit
For g/g；The mass volume ratio of the mixed solution of the PVP-K30 and ethyl alcohol and deionized water composition is 1 ~ 3:100, unit g/
ml。
Further, the mass volume ratio for the mixed solution that above-mentioned trimesic acid and ethyl alcohol are formed with deionized water is
0.6304 ~ 0.8994:100, unit g/ml.
Further, the volume ratio of above-mentioned solution A and solution B is 1:10.
Further, it is above-mentioned based on template construct the preparation of nanometer threadiness manganese selenide/carbon composite be will be obtained above
Nanometer threadiness metal organic framework compound Mn-BTC and selenium powder are individually positioned in the both ends of porcelain boat, and porcelain boat is then placed in pipe
In formula furnace, Mn-BTC is in downstream, and Se powder is in upstream, is that 2 ~ 5 DEG C/min rises to from room temperature with heating rate under an argon atmosphere
400 ~ 600 DEG C, and in 400 ~ 600 DEG C of 2 ~ 4h of heat preservation, obtain nanometer threadiness manganese selenide/carbon composite.
Further, the mass ratio of above-mentioned Mn-BTC and Se powder is 1:1 ~ 10.
The present invention have it is following the utility model has the advantages that
Nano wire prepared by the present invention is not easy to break, and pattern is uniform, good dispersion, is not in agglomeration；The present invention is made
Manganese selenide/carbon composite purity is high, purity may be up to 99.1%；Yield is high, and up to 70% or more；Storage capacity is big, follows
The ring service life is long, in 100mA g-1Current density under after 60 charge and discharge cycles, discharge capacity be 846.59mAh g-1, storage capacity is big, and cycle-index at least can achieve 60 times, at most can up to 200 times, use process stability is good, will not go out
The suddenly big or suddenly small situation of existing electric current, process flow simple possible are worth marketing.
Detailed description of the invention
The SEM figure that Fig. 1 is nanometer threadiness metal organic framework compound Mn-BTC in the embodiment of the present invention.
Fig. 2 is nanometer threadiness manganese selenide/carbon composite SEM figure in the embodiment of the present invention.
Fig. 3 is nanometer threadiness manganese selenide/carbon composite XRD diagram in the embodiment of the present invention.
Fig. 4 is for nanometer threadiness manganese selenide/carbon composite in the embodiment of the present invention as lithium cell negative pole material in 100mA/g
Current density under 60 cyclic curve figures.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment 1:
It is a kind of that nanometer threadiness manganese selenide/carbon composite preparation method is constructed based on MOFs template, comprising the following steps:
1) preparation of nanometer threadiness metal organic framework compound Mn-BTC: 0.2 mmol Mn (CH is weighed3COO)2·4H2O and
350 turns/min of revolving speed, mixing time 8min is arranged in 0.3 g PVP (K30), is dissolved in the mixed of 10 ml ethyl alcohol and deionized water
It closes in solution (v:v=1:1), weighs 0.43 mmol trimesic acid, 350 turns/min of revolving speed is set, mixing time 8min is molten
Solution in 10 ml ethyl alcohol and the mixed solution (v:v=1:1) of deionized water, it is to be mixed be completely dissolved after, use the liquid relief of 1 ml
Rifle is by Mn (CH3COO)2·4H2O solution instills in trimesic acid solution, stirs 10 min, stops aging at room temperature after stirring
Then product is centrifuged 15000 turns/min by 24 h, collect centrifugation, with the mixed solution of ethyl alcohol and deionized water (v:v=1:
1) it washs 3 times, is subsequently placed at 60 DEG C of 12 h of vacuum drying, products therefrom is nanometer threadiness metal organic framework compound Mn-
White is presented in BTC, product, and shape is that nanometer is linear；
2) preparation of nanometer threadiness manganese selenide/carbon composite is constructed based on MOFs template: the nanometer of step 1) preparation is linear
Metal organic framework compound Mn-BTC and Se powder are individually positioned in the both ends of porcelain boat according to the mass ratio of 1:10, then by porcelain boat
It is placed in tube furnace, Mn-BTC is in downstream, and Se powder is in upstream, is 3 DEG C/min from room with heating rate under an argon atmosphere
Temperature rise obtains nanometer threadiness manganese selenide/carbon composite to 450 DEG C, and in 450 DEG C of 3 h of heat preservation.
The nano wire of preparation is not easy to break, and pattern is uniform, good dispersion, does not find agglomeration, while nanometer threadiness selenium
Change manganese/carbon composite, maintain the nanometer threadiness pattern of metal organic framework compound well, crystallinity is high, have compared with
High specific surface area and porosity shows excellent storage lithium performance, and product purity is high, and up to 99.1%.
The results showed that nanometer threadiness manganese selenide/carbon composite prepared by the present invention has excellent storage lithium performance,
In 100mA g-1Current density under after 60 charge and discharge cycles, discharge capacity be 846.59mAh g-1, by experiment
It proves, it is unattenuated to can reach 200 cycle charge-discharges.
Embodiment 2:
It is a kind of to be constructed based on MOFs template as nanometer threadiness manganese selenide/carbon composite preparation method, comprising the following steps:
1) preparation of nanometer threadiness metal organic framework compound Mn-BTC: 0.2 mmol Mn (CH is weighed3COO)2·4H2O and
400 turns/min of revolving speed, mixing time 10min is arranged in 0.3 g PVP (K30), is dissolved in the mixed of 10ml ethyl alcohol and deionized water
It closes in solution (v:v=1:1), weighs 0.43 mmol trimesic acid, 300 turns/min of revolving speed, mixing time 10min are set,
Be dissolved in 10 ml ethyl alcohol and the mixed solution (v:v=1:1) of deionized water, it is to be mixed be completely dissolved after, use the liquid relief of 1ml
Rifle is by Mn (CH3COO)2·4H2O solution instills in trimesic acid solution, stirs 10min, stops aging at room temperature after stirring
For 24 hours, product is then centrifuged 15000 turns/min, collects centrifugation, with the mixed solution of ethyl alcohol and deionized water (v:v=1:
1) it washs 3 times, is subsequently placed at 60 DEG C of vacuum drying 12h, products therefrom is nanometer threadiness metal organic framework compound Mn-
White is presented in BTC, product, and shape is that nanometer is linear；
2) preparation of nanometer threadiness manganese selenide/carbon composite is constructed based on MOFs template: the nanometer of step 1) preparation is linear
Metal organic framework compound Mn-BTC and Se powder are individually positioned in the both ends of porcelain boat according to the mass ratio of 1:6, then by porcelain boat
It is placed in tube furnace, Mn-BTC is in downstream, and Se powder is in upstream, is 2 DEG C/min from room temperature with heating rate under an argon atmosphere
600 DEG C are risen to, and in 600 DEG C of heat preservation 2h, obtains nanometer threadiness manganese selenide/carbon composite.
The nano wire of preparation is not easy to break, and pattern is uniform, good dispersion, does not find agglomeration, while nanometer threadiness selenium
Change manganese/carbon composite, maintain the nanometer threadiness pattern of metal organic framework compound well, crystallinity is high, have compared with
High specific surface area and porosity shows excellent storage lithium performance, and product purity is high, and up to 99.0%, storage capacity is big,
Have extended cycle life, it is 60 times at least recyclable, at most can be recycled 200 times it is unattenuated, use process stability is good, is not in
The suddenly big or suddenly small situation of electric current.
Embodiment 3:
It is a kind of that nanometer threadiness manganese selenide/carbon composite preparation method is constructed based on MOFs template, comprising the following steps:
1) preparation of nanometer threadiness metal organic framework compound Mn-BTC: 0.2 mmol Mn (CH is weighed3COO)2·4H2O and
400 turns/min of revolving speed, mixing time 6min is arranged in 0.3 g PVP (K30), is dissolved in the mixed of 10ml ethyl alcohol and deionized water
It closes in solution (v:v=1:1), weighs 0.43 mmol trimesic acid, 400 turns/min of revolving speed is set, mixing time 6min is molten
Solution in 10 ml ethyl alcohol and the mixed solution (v:v=1:1) of deionized water, it is to be mixed be completely dissolved after, use the liquid-transfering gun of 1ml
By Mn (CH3COO)2·4H2O solution instill trimesic acid solution in, stir 10min, stop stirring after at room temperature aging for 24 hours,
Then product is centrifuged 15000 turns/min, collects centrifugation, product is centrifugated, with the mixing of ethyl alcohol and deionized water
Solution (v:v=1:1) washs 3 times, is subsequently placed at 60 DEG C of vacuum drying 12h, products therefrom is nanometer threadiness metal organic framework
White is presented in compound Mn-BTC, product, and shape is that nanometer is linear；
2) preparation of nanometer threadiness manganese selenide/carbon composite is constructed based on MOFs template: the nanometer of step 1) preparation is linear
Metal organic framework compound Mn-BTC and Se powder are individually positioned in the both ends of porcelain boat according to the mass ratio of 1:8, then by porcelain boat
It is placed in tube furnace, Mn-BTC is in downstream, and Se powder is in upstream, is 5 DEG C/min from room temperature with heating rate under an argon atmosphere
500 DEG C are risen to, and in 450 DEG C of heat preservation 4h, obtains nanometer threadiness manganese selenide/carbon composite.
The nano wire of preparation is not easy to break, and pattern is uniform, good dispersion, does not find agglomeration, while nanometer threadiness selenium
Change manganese/carbon composite, maintain the nanometer threadiness pattern of metal organic framework compound well, crystallinity is high, have compared with
High specific surface area and porosity shows excellent storage lithium performance, and product purity is high, and up to 99.1%, storage capacity is big,
Have extended cycle life, it is 60 times at least recyclable, at most can be recycled 200 times it is unattenuated, use process stability is good, is not in
The suddenly big or suddenly small situation of electric current.
Claims (7)
1. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite, which is characterized in that it is with Mn (CH3COO)2·
4H2O, the mixed solution of PVP-K30, ethyl alcohol and water, trimesic acid, selenium powder are raw material, pass through nanometer metallic threadlike respectively
The preparation of organic framework compounds Mn-BTC constructs nanometer threadiness manganese selenide/carbon composite preparation based on template；
Wherein, the mixed solution of the ethyl alcohol and water is to be obtained by mixing by volume for 1:1.
2. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as described in claim 1, which is characterized in that on
The preparation for stating nanometer threadiness metal organic framework compound Mn-BTC is to take Mn (CH3COO)2·4H2O and PVP-K30 are dissolved in second
300 ~ 400 turns/min of revolving speed is set in the mixed solution of alcohol and deionized water composition, mixing time is 6 ~ 10min, dissolves mixed
Close solution A；Trimesic acid is separately taken to be dissolved in the mixed solution of ethyl alcohol and deionized water composition, 300 ~ 400 turns of revolving speed of setting/
Min, mixing time are 6 ~ 10min, dissolve to obtain solution B；Then solution A is added dropwise in solution B under agitation, is stirred
10min ~ 20min stops stirring, places aging 20 ~ for 24 hours at room temperature, and product is then centrifuged 15000 turns/min, collect from
Then the heart precipitating wash precipitating 3 times with the mixed solution of ethyl alcohol and deionized water, the precipitating and ethyl alcohol and deionized water are mixed
Conjunction liquor capacity ratio is 1:100 ~ 1:150, precipitating is placed in 55 ~ 65 DEG C of air dryings, dry 12 ~ 15h, products therefrom is
White is presented in the linear metal organic framework compound Mn-BTC of nanometer, product, and shape is that nanometer is linear.
3. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as claimed in claim 2, which is characterized in that on
State Mn (CH3COO)2·4H2The mass ratio of O and PVP-K30 is 0.2449 ~ 0.4898:1 ~ 3, unit g/g；The PVP-K30
Mass volume ratio with ethyl alcohol and the mixed solution of deionized water composition is 1 ~ 3:100, unit g/ml.
4. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as claimed in claim 3, which is characterized in that on
The mass volume ratio for stating the mixed solution of trimesic acid and ethyl alcohol and deionized water composition is 0.6304 ~ 0.8994:100, single
Position is g/ml.
5. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as claimed in claim 4, which is characterized in that on
The volume ratio for stating solution A and solution B is 1:10.
6. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as claimed in claim 5, which is characterized in that on
Stating and constructing the preparation of nanometer threadiness manganese selenide/carbon composite based on template is by the organic bone of nanometer metallic threadlike obtained above
Frame compound Mn-BTC and selenium powder are individually positioned in the both ends of porcelain boat, then porcelain boat are placed in tube furnace, Mn-BTC is under
Trip, Se powder is in upstream, under an argon atmosphere, with heating rate is that 2 ~ 5 DEG C/min rises to 400 ~ 600 DEG C from room temperature, and 400 ~
600 DEG C of 2 ~ 4h of heat preservation, obtain nanometer threadiness manganese selenide/carbon composite.
7. the preparation method of a kind of nanometer of linear manganese selenide/carbon composite as claimed in claim 6, which is characterized in that on
The mass ratio for stating Mn-BTC and Se powder is 1:1 ~ 10.
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| CN110364702A (en) * | 2019-06-11 | 2019-10-22 | 杭州电子科技大学 | Chinese chestnut shape is classified application of the manganese selenide/carbon composite as lithium ion battery negative material |
| CN110212161A (en) * | 2019-06-21 | 2019-09-06 | 电子科技大学 | A kind of negative electrode of lithium ion battery and preparation method thereof |
| CN110212161B (en) * | 2019-06-21 | 2022-05-24 | 电子科技大学 | Lithium ion battery cathode and preparation method thereof |
| CN114560448A (en) * | 2022-02-23 | 2022-05-31 | 西安交通大学 | Preparation method and application of manganese selenide nano material |
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