CN109626382A - A kind of preparation method of thermal battery electrolyte carrier - Google Patents

A kind of preparation method of thermal battery electrolyte carrier Download PDF

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Publication number
CN109626382A
CN109626382A CN201910005470.XA CN201910005470A CN109626382A CN 109626382 A CN109626382 A CN 109626382A CN 201910005470 A CN201910005470 A CN 201910005470A CN 109626382 A CN109626382 A CN 109626382A
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CN
China
Prior art keywords
print
battery electrolyte
thermal battery
preparation
egg white
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.)
Pending
Application number
CN201910005470.XA
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Chinese (zh)
Inventor
不公告发明人
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Northwest University
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Northwest University
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Publication date
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Priority to CN201910005470.XA priority Critical patent/CN109626382A/en
Publication of CN109626382A publication Critical patent/CN109626382A/en
Pending legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M6/00—Primary cells; Manufacture thereof
    • H01M6/30—Deferred-action cells
    • H01M6/36—Deferred-action cells containing electrolyte and made operational by physical means, e.g. thermal cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution

Abstract

The invention discloses a kind of preparation methods of thermal battery electrolyte carrier, comprising: step S1 selection, step S2 mixing, step S3 molding, step S4 baking, step S5 calcining, step S6 are cooling；S1: the egg white and deionized water of choosing.The beneficial effects of the invention are as follows, cost of material used in the present invention is low, and process route of the invention is simple, it is easily achieved, higher porosity is easily obtained under high-temperature calcination using this high molecular weight protein of egg white as template and silica, and the better mechanical property of prepared silica matrix carrier structure, there is preferable thermal stability, provides an excellent carrier for the storage of thermal battery electrolyte.

Description

A kind of preparation method of thermal battery electrolyte carrier
Technical field
The present invention relates to thermal battery electrolyte field, especially a kind of preparation method of thermal battery electrolyte carrier.
Background technique
Compared with prior art, the present invention most has the advantages that: cost of material used in the present invention is low, and this hair Bright process route is simple, it is easy to accomplish, using this high molecular weight protein of egg white as template and silica in high temperature Calcining is lower easily to obtain higher porosity, and the better mechanical property of prepared silica matrix carrier structure, has preferably Thermal stability, provide an excellent carrier for the storage of thermal battery electrolyte.
Summary of the invention
Realize above-mentioned purpose the technical scheme is that, a kind of preparation method of thermal battery electrolyte carrier, comprising: step Rapid S1 selection, step S2 mixing, step S3 molding, step S4 baking, step S5 calcining, step S6 are cooling；
S1: egg white and deionized water are chosen；
S2: egg white is added in deionized water, so that titanium dioxide is added after being sufficiently mixed in egg white and deionized water In Si powder, being sufficiently stirred is uniformly dispersed in egg white and water in silica；
S3: evenly dispersed thick solution is transferred to compression molding in compression mold；
S4: print is put into after carrying out the pretreatment regular hour in baking oven and is taken out；
S5: pretreated print is put into tube furnace and calcines the regular hour；
S6: it is taken out after it is cooled to room temperature.
Preferably, content used in egg white described in step S1 is 20~30wt%, and nano silica used contains Amount is 15~25wt%.
Preferably, the pretreated time is 90~110 DEG C to print described in step S4 in an oven.
Preferably, pretreatment time is 20~30min to print described in step S4 in an oven.
Preferably, the temperature that print described in step S5 is calcined in tube furnace is 680~720 DEG C.
Preferably, the calcination time in tube furnace of print described in step S5 is 2~3h.
Preferably, tabletting described in step S3 firmly uniformly will guarantee that drug sheet shaping structures are preferable, inside is without macroscopic view Gap etc..
Using technical solution of the present invention production thermal battery electrolyte carrier preparation method, the present invention used in raw material Process route at low cost and of the invention is simple, it is easy to accomplish, using this high molecular weight protein of egg white as template and Silica easily obtains higher porosity, and the mechanicalness of prepared silica matrix carrier structure under high-temperature calcination Preferably there can be preferable thermal stability, provide an excellent carrier for the storage of thermal battery electrolyte.
Detailed description of the invention
Fig. 1 is thermal cell schematic diagram of internal structure；
Fig. 2 is electrolyte carrier macro morphology figure；
Fig. 3 is electrolyte carrier microscopic appearance figure；
Fig. 4 is the XRD spectrum of print of the present invention；
Fig. 5 is the graph of pore diameter distribution of print of the present invention；
Fig. 6 is the aperture ratio of print of the invention and the relational graph of porosity；
Specific embodiment
The present invention is specifically described with reference to the accompanying drawing, as shown in figures 1 to 6, a kind of system of thermal battery electrolyte carrier Preparation Method.
Embodiment 1:
S1, the egg clear solution of 0.5ml, 0.5ml, 1ml is added in 1.5ml, 2ml, 1.5ml deionized water respectively, made It is sufficiently mixed.
S2, will be sufficiently mixed respectively after solution be added 0.5g nano SiO 2 particle in, being sufficiently stirred makes its mixing Uniformly.
S3, it point will prepare thick solution and be transferred to compression molding in compression mold, and be denoted as print a, print respectively B, print c.
S4, it is put into pretreatment (20min) in baking oven (100 DEG C) after taking out print takes out afterwards.
S5, pretreated print is put into tube furnace (700 DEG C) after calcining (3h), to its in tube furnace it is naturally cold But to taking out after room temperature.
Embodiment 2:
S1,1.5ml egg white is added in 4.5ml deionized water, is mixed them thoroughly.
S2, will be sufficiently mixed after solution be added 1.5g nano SiO 2 particle in, be sufficiently stirred make its be uniformly mixed.
S3, it thick solution will be prepared is transferred to compression molding in compression mold, and the print prepared will be remembered respectively For print d, print e, print f.
S4, it is put into pretreatment (20min) in baking oven (100 DEG C) after successively taking out print takes out afterwards.
S5, pretreated print d, print e, print f are respectively put into tube furnace in 650 DEG C, 700 DEG C, 750 DEG C of conditions After lower calcining 3h, taken out after cooled to room temperature in tube furnace after it.
Embodiment 3:
S1,1.5ml egg white is added in 4.5ml deionized water, is mixed them thoroughly.
S2, will be sufficiently mixed after solution be added 1.5g nano SiO 2 particle in, be sufficiently stirred make its be uniformly mixed.
S3, it thick solution will be prepared is transferred to compression molding in compression mold, and the print prepared will be remembered respectively For print g, print h, print i.
S4, it is put into pretreatment (20min) in baking oven (100 DEG C) after successively taking out print takes out afterwards.
S5, pretreated print g, print h, print i are respectively put into tube furnace calcined under conditions of 700 DEG C 2h, After 3h, 4h, taken out after cooled to room temperature in tube furnace after it.
The parameter of each technique and the selection analysis of process conditions are as follows in the present invention:
1, the influence of the egg clear solution device to hole gap rate of various concentration.
Fig. 1 is the internal structure chart of thermal cell, by previous experiments it is found that when egg white weight percentage 20~ Between 30wt%, preferable hardness and porosity are easily obtained, hole, which can lose print, observes the speed that bubble is bubbled in water Rate and the size of bubble carry out macro-scale characterization.The macro morphology figure of print a carried out by Fig. 2.By comparing print a water suction before and State when water suction, it can be found that when print into the water when there is a large amount of bubble quickly to generate and discharge from the surface of print Out, this is because hydrone enters the inside of print, the gas that the inside is adsorbed in the gap between silica dioxide granule is occupied Body molecule, which is expelled from, to be come, and showing the inside of sample, there are pore structures.
The microscopic appearance of sample surface and inner section can be characterized by SEM image, and Fig. 3 show the microcosmic of print a Shape appearance figure.The SEM image on the surface and section of print a, b, c after measured, through observation shows that: when the content of egg white is When 18wt%, the surface of print and internal hole are smaller, when the mass percentage of quality egg white is increased to 21.6wt% When, hole is increased and aperture is increased, and is distributed relatively uniform；When the mass percentage of egg white is increased to More uniform hole is formd when 35.5wt%, on print.But compare the mechanical performance of print simultaneously, Yi Faxian is with egg white Mass percentage raising, the hardness of print can be gradually reduced.
In order to determine the ingredient of print after calcination at high temperature, XRD test, XRD analysis map such as Fig. 4 have been carried out to print It, will shown in (it is 21.6wt% that wherein a, which is the content of egg white at 650 DEG C, and b is that the content of 700 DEG C of egg whites is 21.6wt%) It with number is that 29-0085 silica coincide after the comparison of the PDF standard card of its XRD spectrum and standard, and the XRD of two samples Map is completely coincident, and illustrates that egg white and moisture thoroughly volatilize by high-temperature calcination processing (when temperature > 650 DEG C).
Its porosity is measured by mercury injection apparatus, and Fig. 5 is the graph of pore diameter distribution of print a and b, and the average pore size of print a is The pore-size distribution of 29.6nm, print b are 27.8nm.Fig. 6 is the relational graph of aperture ratio and porosity, finally measures the hole of print a Gap rate are as follows: the porosity of 75.0657%, print b are 73.6188%.By comparing known to the result of measurement: in certain range The interior mass percentage for improving egg white can improve the porosity of print and appropriate hole diameter enlargement.But work as the quality of egg white When excessively high the mechanical performance of print can decline score, thus will affect the efficiency of thermal cell at work, therefore preferably egg Clear mass percentage is 20wt%~30wt%.
2, influence of the different calcination temperatures to hardness.
Stability between silica is preferable, and when temperature reaches 650 DEG C, the surface of nanometer silicon dioxide particle starts Change, in order to compare influence of the different temperatures to its mechanical performance, the temperature of experimental temperature setting control group of the invention Respectively 650 DEG C, 700 DEG C, 750 DEG C, wherein the mass percent of print each component is respectively as follows: SiO2(19.6wt%), egg (21.6wt%), deionized water (58.8wt%) clearly.
Print Temperature (DEG C) Calcination time (h) Hardness (HRC)
Print d 650 3 12
Print e 700 3 13
Print f 750 3 13
By comparing it is found that hardness increases when temperature reaches 700 DEG C.When temperature continues to rise to 750 DEG C, The hardness of print does not change significantly, therefore preferably experimental temperature is 700 DEG C.
3, influence of the different calcination times to hardness.
The mass percent for the print each component that the experiment of this group uses is respectively as follows: SiO2(19.6wt%), egg white (21.6wt%), deionized water (58.8wt%), calcination temperature are 700 DEG C.At a high temperature of 700 DEG C, egg white and deionization Water thoroughly volatilizees, and different calcination times mainly influences Nano-meter SiO_22The sintering situation of particle surface, macro manifestations are The difference of hardness, specific measurement result see the table below.
Print Calcination time Hardness (HRC)
Print g 2 13
Print h 3 13
Print i 4 13
By comparing it is found that properly increasing calcination time at 700 DEG C to hardness without significantly influencing, therefore preferably Experiment calcination time is 2~3h.
Above-mentioned technical proposal only embodies the optimal technical scheme of technical solution of the present invention, those skilled in the art The principle of the present invention is embodied to some variations that some of them part may be made, belongs to the scope of protection of the present invention it It is interior.

Claims (7)

1. a kind of preparation method of thermal battery electrolyte carrier characterized by comprising step S1 selection, step S2 mixing, step Rapid S3 molding, step S4 baking, step S5 calcining, step S6 are cooling；
S1: egg white and deionized water are chosen；
S2: egg white is added in deionized water, so that silicon dioxide powder is added after being sufficiently mixed in egg white and deionized water In end, being sufficiently stirred is uniformly dispersed in egg white and water in silica；
S3: evenly dispersed thick solution is transferred to compression molding in compression mold；
S4: print is put into after carrying out the pretreatment regular hour in baking oven and is taken out；
S5: pretreated print is put into tube furnace and calcines the regular hour；
S6: it is taken out after it is cooled to room temperature.
2. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S1 Stating content used in egg white is 20~30wt%, and the content of nano silica used is 15~25wt%.
3. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S4 Stating print, the pretreated time is 90~110 DEG C in an oven.
4. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S4 Stating print, pretreatment time is 20~30min in an oven.
5. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S5 Stating the temperature that print is calcined in tube furnace is 680~720 DEG C.
6. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S5 Stating print calcination time in tube furnace is 2~3h.
7. a kind of preparation method of thermal battery electrolyte carrier according to claim 1, which is characterized in that institute in step S3 Stating tabletting firmly uniformly will guarantee that drug sheet shaping structures are preferable, the internal gap etc. without macroscopic view.
CN201910005470.XA 2019-01-03 2019-01-03 A kind of preparation method of thermal battery electrolyte carrier Pending CN109626382A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910005470.XA CN109626382A (en) 2019-01-03 2019-01-03 A kind of preparation method of thermal battery electrolyte carrier

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Application Number Priority Date Filing Date Title
CN201910005470.XA CN109626382A (en) 2019-01-03 2019-01-03 A kind of preparation method of thermal battery electrolyte carrier

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Publication Number Publication Date
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774593A (en) * 2009-01-14 2010-07-14 西南科技大学 Ordered porous silica and silicon carbonitride and preparation method and application thereof
WO2013033847A1 (en) * 2011-09-07 2013-03-14 The Governors Of The University Of Alberta N-doped carbon materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774593A (en) * 2009-01-14 2010-07-14 西南科技大学 Ordered porous silica and silicon carbonitride and preparation method and application thereof
WO2013033847A1 (en) * 2011-09-07 2013-03-14 The Governors Of The University Of Alberta N-doped carbon materials

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
ZHI LI ET AL: "Mesoporous nitrogen-rich carbons derived from protein for ultra-high capacity battery anodes and supercapacitors", 《ENERGY & ENVIRONMENTAL SCIENCE》 *
肖莹: "锂离子电池负极材料的微结构调控及电化学性能研究", 《中国博士学位论文全文数据库》 *

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Application publication date: 20190416

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