CN105280879A - Silica/carbon composite porous electrode and preparation method thereof - Google Patents
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Abstract
The present invention discloses a silica/carbon composite porous electrode and a preparation method thereof. The composite porous electrode is formed by compounding silica and a graphite additive, wherein the graphite additive particles form the continuous phase and the silica is uniformly distributed into the graphite additive particle gaps in the microstructure when the mass percentage of the silica in the composite porous electrode is 30-60%, and the silica forms the continuous phase and the graphite additive particles are uniformly distributed into the silica substrate in the microstructure when the mass percentage of the silica in the composite porous electrode is 60-90%. The preparation method comprises: mixing silica and a dispersing agent to prepare a uniform silica sol, uniformly mixing the silica sol and a graphite additive to prepare a mixed slurry, carrying out drying crushing on the mixed slurry to obtain powder, and preparing the powder into the molding billet material. According to the present invention, the silica/carbon composite porous electrode of the present invention has high porosity, and after the silica/carbon composite porous electrode is subjected to electrolysis, the obtained electrode can be powdered through soaking with water without breaking.
Description
Technical field
The present invention relates to a kind of silicon/carbon dioxide composite porous electrode and preparation method thereof, belong to molten-salt electrolysis technical field.
Background technology
Lithium rechargeable battery because of it possess that good cycle, capacity are high, voltage high and be widely used in multiple industry.It is lower that the lifting of capacity of lithium ion battery is largely limited to insert type negative material capacity, its theoretical capacity of the graphite cathode material that current lithium ion battery extensively adopts only 372mAh/g, therefore Si, Sn and Sb etc. become the better selection of performance of lithium ion battery raising by the high-capacity cathode material of the embedding lithium of alloying.Wherein silicon has high power capacity (theoretical capacity 4200mAh/g), low embedding lithium voltage, the advantage such as rich content in the earth's crust.But silicon poor electric conductivity and produce serious bulk effect (volume change is 280% ~ 310%) in removal lithium embedded process, therefore as showing relatively poor cycle life and coulombic efficiency during negative material.It is by silicon nanometer that the way that current people propose to address this problem mainly contains two kinds: one; Two is adopt silicon composite.In many silicon based anode materials, silicon/carbon composite is the focus of this type of research.
The method preparing silicon/carbon composite at present mainly contains the methods such as chemical vapour deposition technique, thermal vapor deposition method, high-energy ball milling.These preparation methods or relate to complex technical process (as template), or process is difficult to control, or equipment needed thereby costliness (as chemical vapour deposition technique), be difficult to realize batch production.Patent documentation CN103107315A discloses a kind of nano-silicone wire/carbon composite material and preparation method thereof, by the method for molten-salt electrolysis, silicon/carbon dioxide composite material is reduced to silicon/carbon composite, achieves the batch preparation of Si-C composite material.Combine between silicon and carbon better in silicon/carbon composite prepared by the method original position, not easily separated as silicon and carbon in doff lithium process during lithium ion battery negative material, make this type of material have the advantage of good cycling stability.
Molten-salt electrolysis a kind of the method for electrolysis is carried out in the salt melting of some metal as electrolyte, is mainly used in extracting and purify metals.Current fused salt electrolysis process is mainly used in the production of the metals such as aluminium.Along with the development of molten-salt electrolysis technique, present the method also can be applied to the production of titanium, Si-C composite material etc.The factor affecting Molten mainly can be divided into two large classes: electrode and electrolysis process (electrolytic potential, electrolysis temperature, electrolysis time and molten salt system etc.), and therefore optimizing technology for preparing electrode, improving electrode performance is an importance in molten-salt electrolysis research.Molten-salt electrolysis electrode adopts dusty material mostly, comprising electro-active powders material (powder itself participates in electrochemical reaction) and powder additive (powder itself does not participate in electrochemical reaction) etc.The electrode prepared by forming material powder has certain porosity mostly, is therefore called " porous electrode ".The major advantage of porous electrode has the reaction surface more much bigger than plate electrode, is conducive to the carrying out of electrochemical reaction.The main structure parameters of characterizing porous electrode comprises than porosity and surface area.In addition, in porous electrode, species distribution also has considerable influence to electrolytic process and product property structure.Nonconducting reactivity material contributes to obtaining continuous print linear structure in product when forming continuous phase, and contributes to the electric conductivity improving porous electrode when inactive conductive materials forms continuous phase, improves electrolysis speed.At present, preparing in the method for Si-C composite material above by fused salt electrolysis process, there is no good porous electrode preparation method.
Summary of the invention
The object of the invention is to prepare Si-C composite material for fused salt electrolysis process and a kind of silicon/carbon dioxide composite porous electrode of good performance is provided, this silicon/carbon dioxide composite porous electrode has the feature of high porosity, and the i.e. pulverizable that is soaked in water after electrolysis, without the need to fragmentation.
Another object of the present invention is to the preparation method providing a kind of described silicon/carbon dioxide composite porous electrode, can realize the control to this porous electrode microstructure by adjustment dioxide-containing silica, the method is simple.
For achieving the above object, the present invention is by the following technical solutions:
A kind of silicon/carbon dioxide composite porous electrode, be composited by silicon dioxide and graphite additive, when the mass percent that silicon dioxide is shared in this composite porous electrode is 30 ~ 60%, in its microstructure, graphite additive particle forms continuous phase, and silicon dioxide is evenly distributed in graphite additive particulate interspaces; And when the mass percent that silicon dioxide is shared in this composite porous electrode is 60 ~ 90%, in its microstructure, silicon dioxide forms continuous phase, graphite additive uniform particles is distributed in silica substrate.
Silicon/carbon dioxide composite porous electrode of the present invention, when the mass percent that silicon dioxide is shared in this composite porous electrode is 30 ~ 60%, its porosity is 30 ~ 60%, is: the porous electrode of compression molding according to different forming method parameter, and porosity is 50 ~ 60%; The porous electrode of isostatic compaction, porosity is 40 ~ 60%; Hot-forming porous electrode, porosity is 30 ~ 50%, the resistivity≤5 Ω cm of this porous electrode; When the mass percent that silicon dioxide is shared in this composite porous electrode is 60 ~ 90%, its porosity is 10 ~ 50%, is: the porous electrode of compression molding according to different forming method parameter, and porosity is 40 ~ 50%; The porous electrode of isostatic compaction, porosity is 30 ~ 50%; Hot-forming porous electrode, porosity is 10 ~ 30%, the resistivity >=5 Ω cm of this porous electrode.
The porosity distribution scope of silicon/carbon dioxide composite porous electrode of the present invention is narrower, only there is 1 ~ 2 peak in the pore size distribution curve tested by mercury injection method.Adhesion between the shaping main dependence silica dioxide granule of silicon/carbon dioxide composite porous electrode of the present invention, the silica dioxide granule volume contraction of this porous electrode in electroreduction rear electrode, structure changes, therefore, porous electrode of the present invention is soaked in water remove molten salt electrolyte rear electrode residual in electrode can efflorescence voluntarily, without the need to fragmentation.
In the present invention, described silicon dioxide is the silicon dioxide that vapor phase method or coprecipitation are produced, its purity >=99%.Described graphite additive be lithium ion battery graphite cathode material, the agent of lithium ion battery graphite, high-purity natural graphite and other carbon, graphite material one or more.When additive is two or more, between each component, there is no limited proportion.
A preparation method for described silicon/carbon dioxide composite porous electrode, at least comprises the following steps:
The first step: be (0.10 ~ 0.40) in mass ratio by silicon dioxide and dispersant: 1 is mixed with uniformly silicon dioxide gel; This step can be carried out in planetary stirring machine, and planetary stirring machine rotation is stirred and is not less than 50rpm with revolution speed of agitator.
Second step: by the silicon dioxide gel obtained and graphite additive be in mass ratio (1.5 ~ 10): 1 mixes and makes mixed slurry; This step can be carried out in planetary stirring machine, and planetary stirring machine rotation is stirred and is not less than 50rpm with revolution speed of agitator, also can carry out in banbury or twin screw compounder.
3rd step: by mixed slurry under 80 ~ 120 DEG C of environment dry 12 ~ 48 hours, be then ground into the powder of granularity≤1mm, and powder is made shaping blank.
In this preparation method, described dispersant can be water, gasoline, alcohols, ketone or ester class.The forming method of powder can select mold pressing or mould to fill with shaping, isostatic compaction or hot-forming.The pressure of compression molding is 0.5 ~ 30MPa, is preferably 2 ~ 30MPa; Dwell time is 1 ~ 20min, is preferably 5 ~ 10min.The pressure of isostatic compaction is 100 ~ 200MPa; Dwell time is 1 ~ 20min, is preferably 5 ~ 10min.Hot-forming temperature is 800 ~ 1400 DEG C, is preferably 900 ~ 1300 DEG C; Pressure is 5 ~ 100MPa, is preferably 5 ~ 50MPa; Dwell time is 15 ~ 300min, is preferably 60 ~ 120min.
The invention has the advantages that:
Silicon/carbon dioxide composite porous electrode of the present invention has the feature of high porosity, and the i.e. pulverizable that is soaked in water after electrolysis, without the need to fragmentation.
The preparation method of silicon/carbon dioxide composite porous electrode of the present invention, device therefor is conventional industrial equipment and range of choice is wider, and flow and method is simple; Use raw material to be large-scale industry product, with low cost.
Accompanying drawing explanation
The micro-structure diagram of the porous electrode of Fig. 1 prepared by embodiment 1.
The porosity distribution of the porous electrode of Fig. 2 prepared by embodiment 1.
The micro-structure diagram of the porous electrode of Fig. 3 prepared by embodiment 2.
The porosity distribution of the porous electrode of Fig. 4 prepared by embodiment 2.
The micro-structure diagram of the porous electrode of Fig. 5 prepared by embodiment 3.
The porosity distribution of the porous electrode of Fig. 6 prepared by embodiment 3.
The micro-structure diagram of the porous electrode of Fig. 7 prepared by embodiment 4.
The porosity distribution of the porous electrode of Fig. 8 prepared by embodiment 4.
The micro-structure diagram of the porous electrode of Fig. 9 prepared by embodiment 5.
The porosity distribution of the porous electrode of Figure 10 prepared by embodiment 5.
The micro-structure diagram of the porous electrode of Figure 11 prepared by embodiment 6.
The porosity distribution of the porous electrode of Figure 12 prepared by embodiment 6.
Embodiment
The invention will be further described by the following examples, but the present invention is not limited to following examples.
Embodiment 1
A kind of silicon/carbon dioxide composite porous electrode, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide in the composite mass fraction is 50%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is silicon/carbon/graphite in lithium ion batteries conductive agent KS6, D90 is 6 μm.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 15kg deionized water in the stirred vessel of 60L to volume, and be that the silicon dioxide of 7.5kg divides 4 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, again adds deionized water 15kg in stirred vessel, and is that the KS6 of 7.5kg divides 2 times to add stirred vessel by quality, and add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 120min after adding all KS6, stir speed (S.S.) is 50rpm.
3rd step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
4th step, carries out isostatic compaction to obtained silicon dioxide and KS6 mixture powder material and forms blank isostatic compaction, pressure 175MPa, dwell time 5min.
5th step, is processed into porous electrode by the blank of formation.
In above-mentioned porous electrode microstructure, KS6 particle forms continuous conduction phase, and silicon dioxide is distributed between KS6 particle, and therefore this porous electrode has lower resistivity (0.1-0.2 Ω cm), and its microstructure as shown in Figure 1.Test porosity and the discovery of pore-size distribution situation thereof of this porous electrode by mercury injection method, this electrode porosity is 46.6%, only has a peak, as shown in Figure 2 in its porosity distribution curve.
Embodiment 2
A kind of silicon/carbon dioxide composite porous electrode, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide in the composite mass fraction is 70%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is lithium ion battery negative material 918, D90 is 6 μm.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 1800g deionized water in the stirred vessel of 6L to volume, and be that the silicon dioxide of 700g divides 6 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, in stirred vessel, add quality is continue behind 918 of 300g to stir 120min, and stir speed (S.S.) is 50rpm.
3rd step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
4th step, carry out hot-forming formation blank to obtained silicon dioxide and 918 mixture powder material, hot-forming temperature is 1200 DEG C, pressure 7MPa, dwell time 75min.
5th step, is processed into porous electrode by the blank of formation.
In above-mentioned porous electrode microstructure, nano silicon forms continuous phase, and 918 distribution of particles are between nano silicon, and therefore this porous electrode resistivity is higher, and its mean value reaches 70.3 Ω cm, and its microstructure as shown in Figure 3.Test porosity and the discovery of pore-size distribution situation thereof of this porous electrode by mercury injection method, this electrode porosity is 20.4%, only has 2 obvious peaks, as shown in Figure 4 in its porosity distribution curve.
Embodiment 3
A kind of silicon/carbon dioxide composite porous electrode and preparation method thereof, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide mass fraction is in the composite 50%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is lithium ion battery negative material 918, D90 is 28 μm.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 15kg deionized water in the stirred vessel of 60L to volume, and be that the silicon dioxide of 7.5kg divides 4 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, again adds deionized water 15kg in stirred vessel, and is that 918 points of 7.5kg add stirred vessel 2 times by quality, and add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue after adding all 918 to stir 120min, stir speed (S.S.) is 50rpm.
3rd step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
4th step, carry out hot-forming formation blank to obtained silicon dioxide and 918 mixture powder material, hot-forming temperature is 1100 DEG C, pressure 7MPa, dwell time 75min.
5th step, is processed into porous electrode by the blank of formation.
In its microstructure of gained silicon/carbon dioxide composite porous electrode, 918 particles form continuous conduction phase as stated above, and silicon dioxide is distributed between 918 particles, therefore this porous electrode has lower resistivity (1.5-2.0 Ω cm), and its microstructure as shown in Figure 5.Fig. 6 is the pore-size distribution of this porous electrode recorded by mercury injection method, and this porous electrode pore size distribution curve only has 2 obvious peaks as we can see from the figure, and this electrode porosity reaches 42.2%, bulk density 1.32g/cm3 in addition.
Embodiment 4
A kind of silicon/carbon dioxide composite porous electrode and preparation method thereof, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide in the composite shared mass ratio is 40%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is bi-material mixture, and one be lithium ion battery negative material 918, D90 is 28 μm, and another kind is graphitized carbon fibre VGCF, and the mass ratio of the two is 29: 1.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 1.5kg deionized water in the stirred vessel of 15L to volume, and be that the silicon dioxide of 400g divides 4 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, again adds deionized water 1.5kg in stirred vessel, and be that 918 points of 580g add stirred vessel 2 times by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn.
3rd step, be that the graphitized carbon fibre VGCF of 20g adds stirred vessel by quality, and stir 120min, stir speed (S.S.) is 50rpm.
4th step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
5th step, carry out hot-forming formation blank to obtained silicon dioxide and 918 mixture powder material, hot-forming temperature is 1100 DEG C, pressure 7MPa, dwell time 75min.
6th step, is processed into porous electrode by the blank of formation.
The silicon/carbon dioxide composite porous electrode prepared as stated above: porosity 43.9%, average resistivity is 0.53 Ω cm.In its microstructure, 918 particles form continuous conduction phase, silicon dioxide is distributed between 918 particles, and the existence of graphitized carbon fibre VGCF enhances the connection between 918 particles, reduce further the resistivity of porous electrode, this porous electrode electron micrograph as shown in Figure 7.As shown in Figure 8, as we can see from the figure, in this porous electrode pore size distribution curve, only there are 2 peaks in the pore size distribution curve of this porous electrode.
Embodiment 5
A kind of silicon/carbon dioxide composite porous electrode and preparation method thereof, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide in the composite mass fraction is 50%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is silicon/carbon/graphite in lithium ion batteries conductive agent KS6, D90 is 6 μm.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 15kg deionized water in the stirred vessel of 60L to volume, and be that the silicon dioxide of 7.5kg divides 4 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, again adds deionized water 15kg in stirred vessel, and is that the KS6 of 7.5kg divides 3 times to add stirred vessel by quality, and add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue after adding all 918 to stir 120min, stir speed (S.S.) is 50rpm.
3rd step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
4th step, carries out isostatic compaction, hydrostatic pressure 185MPa, dwell time 5min to obtained silicon dioxide and KS6 mixture powder material.
5th step, is processed into the blank machine that isostatic pressed obtains the nano silicon/KS6 composite porous electrode being of a size of 100 × 100 × 5mm.
Gained silicon/carbon dioxide composite porous electrode: porosity 50.3%, resistivity distribution is at 150-200m Ω cm, and in its microstructure, KS6 particle forms continuous conduction phase, and silicon dioxide is distributed between KS6 particle, and its microstructure as shown in Figure 9.Can see only there is a peak in curve from the pore size distribution curve of Figure 10.
Embodiment 6
A kind of silicon/carbon dioxide composite porous electrode and preparation method thereof, its raw material comprises silicon dioxide and graphite additive, and silicon dioxide in the composite mass fraction is 50%, and described silicon dioxide is: nano silicon prepared by vapor phase method, particle diameter is 30 ± 5nm, purity >=99.5%; Described graphite additive is silicon/carbon/graphite in lithium ion batteries conductive agent KS6, D90 is 6 μm.
The preparation method of this silicon/carbon dioxide composite porous electrode comprises the following steps:
The first step is add 15kg deionized water in the stirred vessel of 60L to volume, and be that the silicon dioxide of 7.5kg divides 4 times to add in stirred vessel by quality, add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue to stir 60min after adding all silicon dioxide, stir speed (S.S.) is 50rpm.
Second step, again adds deionized water 15kg in stirred vessel, and is that the KS6 of 7.5kg divides 3 times to add stirred vessel by quality, and add rear stirring 3min, stir speed (S.S.) is 50rpm at every turn; Continue after adding all 918 to stir 120min, stir speed (S.S.) is 50rpm.
3rd step, by the mixed slurry after stirring under 120 DEG C of environment dry 24 hours, then pulverizes the powder for granularity≤1mm.
4th step, carries out isostatic compaction, hydrostatic pressure 185MPa, dwell time 5min to obtained silicon dioxide and KS6 mixture powder material.
5th step, is processed into size 100 × 100 × 5mm by the blank machine that isostatic pressed obtains.
6th step, by the porous electrode after processing at 1100 DEG C, sinters 1 hour under nitrogen atmosphere.
Gained silicon/carbon dioxide composite porous electrode: porosity 40.03%, average resistivity 83m Ω cm, in its microstructure, KS6 particle forms continuous conduction phase, and silicon dioxide is distributed between KS6 particle, and its microstructure as shown in figure 11.Can see only there is a peak in curve from the pore size distribution curve of Figure 12.
Claims (13)
1. a silicon/carbon dioxide composite porous electrode, is characterized in that: this composite porous electrode is composited by silicon dioxide and graphite additive; The mass percent of silicon dioxide shared by this composite porous electrode is 30 ~ 60%; In its microstructure, graphite additive particle forms continuous phase, and silicon dioxide is evenly distributed in graphite additive particulate interspaces.
2. a silicon/carbon dioxide composite porous electrode, is characterized in that: this composite porous electrode is composited by silicon dioxide and graphite additive; The mass percent of silicon dioxide shared by this composite porous electrode is 60 ~ 90%; In its microstructure, silicon dioxide forms continuous phase, and graphite additive uniform particles is distributed in silica substrate.
3. silicon/carbon dioxide composite porous electrode according to claim 1, is characterized in that: its porosity is 30 ~ 60%, its resistivity≤5 Ω cm.
4. silicon/carbon dioxide composite porous electrode according to claim 2, is characterized in that: its porosity is 10 ~ 50%, its resistivity >=5 Ω cm.
5. silicon/carbon dioxide composite porous electrode according to claim 1 and 2, is characterized in that: the porosity distribution scope of described porous electrode is narrower, only there is 1 ~ 2 peak with in the pore size distribution curve of mercury injection method test.
6. silicon/carbon dioxide composite porous electrode according to claim 1 and 2, is characterized in that: described silicon dioxide is the silicon dioxide that vapor phase method or coprecipitation are produced, its purity >=99%.
7. silicon/carbon dioxide composite porous electrode according to claim 1 and 2, is characterized in that: described graphite additive be lithium ion battery graphite cathode material, the agent of lithium ion battery graphite, high-purity natural graphite and other carbon, graphite material one or more.
8. a preparation method for the silicon/carbon dioxide composite porous electrode according to any one of claim 1 ~ 7, is characterized in that: at least comprise the following steps:
The first step: be (0.10 ~ 0.40) in mass ratio by silicon dioxide and dispersant: 1 is mixed with uniformly silicon dioxide gel;
Second step: by the silicon dioxide gel obtained and graphite additive be in mass ratio (1.5 ~ 10): 1 mixes and makes mixed slurry;
3rd step: by mixed slurry under 80 ~ 120 DEG C of environment dry 12 ~ 48 hours, be then ground into the powder of granularity≤1mm, and powder is made shaping blank.
9. the preparation method of silicon/carbon dioxide composite porous electrode according to claim 8, is characterized in that: described dispersant is water, gasoline, alcohols, ketone or ester class.
10. the preparation method of silicon/carbon dioxide composite porous electrode according to claim 8, is characterized in that: the forming method of described powder is that mold pressing or mould fill with shaping, isostatic compaction or hot-forming.
The preparation method of 11. silicon/carbon dioxide composite porous electrodes according to claim 10, is characterized in that: the pressure of described compression molding is 0.5 ~ 30MPa, and the dwell time is 1 ~ 20min.
The preparation method of 12. silicon/carbon dioxide composite porous electrodes according to claim 10, is characterized in that: the pressure of described isostatic compaction is 100 ~ 200MPa, and the dwell time is 1 ~ 20min.
The preparation method of 13. silicon/carbon dioxide composite porous electrodes according to claim 10, is characterized in that: described hot-forming temperature is 800 ~ 1400 DEG C, and pressure is 5 ~ 100MPa, and the dwell time is 15 ~ 300min.
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| CN111994912B (en) * | 2020-08-31 | 2022-03-18 | 上海三棵树防水技术有限公司 | Silica sol, silica sol gel composite rock wool thermal insulation material and preparation method thereof |
| WO2023134366A1 (en) * | 2022-01-14 | 2023-07-20 | 广东邦普循环科技有限公司 | Silicon-carbon negative electrode material, and preparation method therefor and use thereof |
| GB2619868A (en) * | 2022-01-14 | 2023-12-20 | Guangdong Brunp Recycling Technology Co Ltd | Silicon-carbon negative electrode material, and preparation method therefor and use thereof |
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