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CN105047430A - Preparation method for portable minitype clean-energy storage device - Google Patents

Preparation method for portable minitype clean-energy storage device Download PDF

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CN105047430A
CN105047430A CN201510415612.1A CN201510415612A CN105047430A CN 105047430 A CN105047430 A CN 105047430A CN 201510415612 A CN201510415612 A CN 201510415612A CN 105047430 A CN105047430 A CN 105047430A
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preparation
concentration
memory device
collector
clean energy
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CN105047430B (en
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赵九蓬
王晶
李垚
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

The invention provides a preparation method for a portable minitype clean-energy storage device, relates to a preparation method for the portable minitype clean-energy storage device, and is to solve a problem that the existing lithium ion battery and supercapacitor materials cannot simultaneously achieve low cost, stability and excellent rate capability. The preparation method comprises the steps: 1, cleaning a current collector; 2, preparing a current collector, wherein cobalt oxide grows on the surface of the current collector; 3, preparing a current collector, wherein the cobalt oxide and cobalt molybdate grow on the surface of the current collector; 4, mixing PVA and KOH, and putting the mixture into water to stir, thereby obtaining a mixed solution C; 5, arranging a fiber resin diaphragm between two current collectors, on the surfaces of which the cobalt oxide and the cobalt molybdate grow, to obtain a component; immersing the component into the mixed solution C, drying the immersed component, and coating the exterior of the dried component with a metal housing, thereby obtaining the portable minitype clean-energy storage device. The preparation method for the portable minitype clean-energy storage device can provide clean energy for electrochromic smart windows, mobile phones, electric vehicles and the like.

Description

The preparation method of the miniature memory device of a kind of portable clean energy
Technical field
The present invention relates to the preparation method of the miniature memory device of a kind of portable clean energy.
Background technology
Along with people are to the continuous demand of the energy, and environmental pollution increasingly sharpens, and development high energy storage, reusable edible, non-environmental-pollution, portable micro power source memory device will become study hotspot.For the development and utilization of the energy, what people used at present has wind energy, water energy, solar energy, tidal energy, electric energy etc.But electric energy, compared with other energy, can in all case use, without the need to the restriction of external environment.Lithium ion battery and ultracapacitor, as the storage device of electric energy, have respective superiority and shortage part.Lithium ion battery can provide high energy density, but power density is but less than ultracapacitor.At present, the research of people how to reduce volumetric expansion, and the specific area and the conductivity that increase material improve its power density, and service life cycle.On the contrary, ultracapacitor has high power density, and longer service life cycle, but along with low energy density.People's report be by improving specific capacity and the voltage window scope of application thus improving its energy density.But by selecting the material having lithium electricity and super electrical property concurrently, the electrical energy storage device being realized high-energy-density and high power density by control condition parameter will solve above-mentioned lithium electricity and super electric produced problem place.For the selection of material, rich content, affordable, and excellent performance.
Cobalt oxide and cobalt molybdate have lithium electricity and super electric performance concurrently, and cobalt element earth rich reserves, cheap.Cobalt oxide, as lithium electricity and super electric material, have high theoretical specific capacity, but stability and high rate performance is but nothing like cobalt molybdate.Therefore, homogenous material can not the diversified modern Application field of content with funtion.
Summary of the invention
The present invention will solve the problem that existing lithium electricity and super electric material can not meet cheap, stability and high rate performance excellence simultaneously, and provides the preparation method of the miniature memory device of a kind of portable clean energy.
The preparation method of the miniature memory device of a kind of portable clean of the present invention energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 5min ~ 120min, then ethanol ultrasonic cleaning 5min ~ 300min is placed in, finally be placed in dilute hydrochloric acid solution ultrasonic cleaning 5min ~ 200min that concentration is 0.01mol/L ~ 6mol/L, obtain clean collector;
Two, be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration by concentration be stir 5min ~ 720min after the urea liquid mixing of 0.0001mol/L ~ 1mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be after heating 0.5h ~ 72h under the condition of 90 DEG C ~ 200 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration the be urea liquid of 0.0001mol/L ~ 1mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration by concentration be stir 5min ~ 720min after the sodium molybdate solution mixing of 0.0001mol/L ~ 3mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be after heating 0.5h ~ 48h under the condition of 90 DEG C ~ 220 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration the be sodium molybdate solution of 0.0001mol/L ~ 3mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 1h ~ 96h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:(1 ~ 30);
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 1min ~ 120min, is then dry 1h ~ 72h in the baking oven of 40 DEG C ~ 120 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
Beneficial effect of the present invention is:
The present invention by two or more materials are carried out compound, and designs a special structure, to realize the multifunctional application of material, improves the weak point of homogenous material according to cooperative effect.Again the composite material of this excellent performance is prepared into required size, is assembled into solid state device form, light weight, is easy to carry.The preparation technology of material is simple, is easy to operation, and material can direct growth and be evenly distributed on collector, and without the need to the use of any additive and masterplate, both environmental protection turn improved the satisfactory electrical conductivity of material and collector.The constructing and prepare easy of this miniature memory device, operability is good, is easy to industrialization.In this experiment, this memory device part achieves and provides electric energy to electrochromic device, realizes the change of the color of electrochromic material.
Accompanying drawing explanation
Fig. 1 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment one obtains;
Fig. 2 is the discharge curve that the miniature memory device of the portable clean energy that embodiment one obtains does under current density 5 amperes of/gram of conditions;
Fig. 3 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment one obtains is powered to electrochromic material molybdenum oxide device; Wherein 1 is coloured state, and 2 is states of fading;
Fig. 4 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment two obtains;
Fig. 5 is the discharge curve that the miniature memory device of the portable clean energy that embodiment two obtains does under current density 6 amperes of/gram of conditions;
Fig. 6 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment two obtains is powered to electrochromic material molybdenum oxide device; Wherein 1 is coloured state, and 2 is states of fading;
Fig. 7 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment three obtains;
Fig. 8 is the discharge curve that the miniature memory device of the portable clean energy that embodiment three obtains does under current density 8 amperes of/gram of conditions;
Fig. 9 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment three obtains is powered to electrochromic material molybdenum oxide device; Wherein 1 is coloured state, and 2 is states of fading.
Embodiment
Embodiment one: present embodiment is that the preparation method of the miniature memory device of a kind of portable clean energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 5min ~ 120min, then ethanol ultrasonic cleaning 5min ~ 300min is placed in, finally be placed in dilute hydrochloric acid solution ultrasonic cleaning 5min ~ 200min that concentration is 0.01mol/L ~ 6mol/L, obtain clean collector;
Two, be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration by concentration be stir 5min ~ 720min after the urea liquid mixing of 0.0001mol/L ~ 1mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be after heating 0.5h ~ 72h under the condition of 90 DEG C ~ 200 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration the be urea liquid of 0.0001mol/L ~ 1mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration by concentration be stir 5min ~ 720min after the sodium molybdate solution mixing of 0.0001mol/L ~ 3mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be after heating 0.5h ~ 48h under the condition of 90 DEG C ~ 220 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration the be sodium molybdate solution of 0.0001mol/L ~ 3mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 1h ~ 96h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:(1 ~ 30);
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 1min ~ 120min, is then dry 1h ~ 72h in the baking oven of 40 DEG C ~ 120 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
The assembly of three-decker described in present embodiment step 5 can be cut into required size and shape according to actual needs.
Present embodiment by two or more materials are carried out compound, and designs a special structure, to realize the multifunctional application of material, improves the weak point of homogenous material according to cooperative effect.Again the composite material of this excellent performance is prepared into required size, is assembled into solid state device form, light weight, is easy to carry.The preparation technology of material is simple, is easy to operation, and material can direct growth and be evenly distributed on collector, and without the need to the use of any additive and masterplate, both environmental protection turn improved the satisfactory electrical conductivity of material and collector.The constructing and prepare easy of this miniature memory device, operability is good, is easy to industrialization.In this experiment, this memory device part achieves and provides electric energy to electrochromic device, realizes the change of the color of electrochromic material.
Embodiment two: present embodiment and embodiment one unlike: be placed in the dilute hydrochloric acid solution ultrasonic cleaning 40min that concentration is 0.08mol/L in step one.Other are identical with embodiment one.
Embodiment three: present embodiment and embodiment one or two unlike: be heat 1h under the condition of 100 DEG C in temperature in step 2.Other are identical with embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three unlike: be heat 2h under the condition of 110 DEG C in temperature in step 2.Other are identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four unlike: be heat 0.8h under the condition of 100 DEG C in temperature in step 3.Other are identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five unlike: the volume ratio of PVA and KOH described in step 4 is 1:3.Other are identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six unlike: the volume ratio of PVA and KOH described in step 4 is 1:8.Other are identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven unlike: be dry 24h in the baking oven of 60 DEG C in temperature in step 5.Other are identical with one of embodiment one to seven.
Beneficial effect of the present invention is verified by following examples:
Embodiment one: the preparation method of the miniature memory device of a kind of portable clean energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 10min, is then placed in ethanol ultrasonic cleaning 5min, is finally placed in the dilute hydrochloric acid solution ultrasonic cleaning 20min that concentration is 0.05mol/L, obtains clean collector;
Two, be the cobalt nitrate solution of 0.0005mol/L and concentration by concentration be stir 30min after the urea liquid mixing of 0.05mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be, after heating 1h under the condition of 100 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0005mol/L and concentration the be urea liquid of 0.05mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.05mol/L and concentration by concentration be stir 10min after the sodium molybdate solution mixing of 0.003mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be, after heating 0.5h under the condition of 90 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.05mol/L and concentration the be sodium molybdate solution of 0.003mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 3h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:1;
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 5min, is then dry 1h in the baking oven of 50 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
Embodiment two: the preparation method of the miniature memory device of a kind of portable clean energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 20min, is then placed in ethanol ultrasonic cleaning 8min, is finally placed in the dilute hydrochloric acid solution ultrasonic cleaning 40min that concentration is 0.08mol/L, obtains clean collector;
Two, be the cobalt nitrate solution of 0.005mol/L and concentration by concentration be stir 40min after the urea liquid mixing of 0.5mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be, after heating 2h under the condition of 110 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.005mol/L and concentration the be urea liquid of 0.5mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.03mol/L and concentration by concentration be stir 30min after the sodium molybdate solution mixing of 0.006mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be, after heating 0.8h under the condition of 100 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.03mol/L and concentration the be sodium molybdate solution of 0.006mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 3h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:3;
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 3min, is then dry 1.5h in the baking oven of 60 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
Embodiment three: the preparation method of the miniature memory device of a kind of portable clean energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 25min, is then placed in ethanol ultrasonic cleaning 15min, is finally placed in the dilute hydrochloric acid solution ultrasonic cleaning 25min that concentration is 0.08mol/L, obtains clean collector;
Two, be the cobalt nitrate solution of 0.004mol/L and concentration by concentration be stir 45min after the urea liquid mixing of 0.07mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be, after heating 3h under the condition of 130 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.004mol/L and concentration the be urea liquid of 0.07mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.09mol/L and concentration by concentration be stir 40min after the sodium molybdate solution mixing of 0.006mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be, after heating 8h under the condition of 150 DEG C, taken out by product from reactor in temperature, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.09mol/L and concentration the be sodium molybdate solution of 0.006mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 12h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:8;
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 5min, is then dry 24h in the baking oven of 65 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
Fig. 1 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment one obtains; This figure can find out, curve does not present rectangle, illustrates that this material is fake capacitance material.
Fig. 2 is the discharge curve that the miniature memory device of the portable clean energy that embodiment one obtains does under current density 5 amperes of/gram of conditions; As can be seen from the figure discharge time is 180s, and voltage is 1.4V.The specific capacity C that can be calculated material by the computing formula C=it/mV of specific capacity is 642 farads/gram.
Fig. 3 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment one obtains is powered to electrochromic material molybdenum oxide device, and wherein 1 is coloured state, and 2 is states of fading; As can be seen from the figure be changed to 50% in the transmitance of 550 nanometers, the performance achieving and power to electrochromic device is described, can be used as energy storage equipment.
Fig. 4 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment two obtains; Can be found out by this figure, curve does not present rectangle, illustrates that this material is fake capacitance material.
Fig. 5 is the discharge curve that the miniature memory device of the portable clean energy that embodiment two obtains does under current density 6 amperes of/gram of conditions; As can be seen from the figure discharge time is 160s, and voltage is 1.5V.The specific capacity C that can be calculated material by the computing formula C=it/mV of specific capacity is 640 farads/gram.
Fig. 6 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment two obtains is powered to electrochromic material molybdenum oxide device, and wherein 1 is coloured state, and 2 is states of fading; Can find out and be changed to 40% in the transmitance of 550 nanometers, the performance achieving and power to electrochromic device is described, can be used as energy storage equipment.
Fig. 7 is the cyclic voltammetry curve of the miniature memory device of the portable clean energy that embodiment three obtains; Can be found out by this figure, curve does not present rectangle, illustrates that this material is fake capacitance material.
Fig. 8 is the discharge curve that the miniature memory device of the portable clean energy that embodiment three obtains does under current density 8 amperes of/gram of conditions; As can be seen from the figure discharge time is 175s, and voltage is 1.6V.The specific capacity C that can be calculated material by the computing formula C=it/mV of specific capacity is 875 farads/gram.
Fig. 9 is the transmitance variation diagram after the miniature memory device of the portable clean energy that embodiment three obtains is powered to electrochromic material molybdenum oxide device, and wherein 1 is coloured state, and 2 is states of fading; Can find out and be changed to 20% in the transmitance of 550 nanometers, the performance achieving and power to electrochromic device is described, can be used as energy storage equipment.

Claims (8)

1. a preparation method for the miniature memory device of the portable clean energy, is characterized in that the preparation method of the miniature memory device of the portable clean energy is undertaken by following steps:
One, the cleaning of collector: collector is placed in water ultrasonic cleaning 5min ~ 120min, then ethanol ultrasonic cleaning 5min ~ 300min is placed in, finally be placed in dilute hydrochloric acid solution ultrasonic cleaning 5min ~ 200min that concentration is 0.01mol/L ~ 6mol/L, obtain clean collector;
Two, be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration by concentration be stir 5min ~ 720min after the urea liquid mixing of 0.0001mol/L ~ 1mol/L, obtain mixed solution A, the collector of cleaning step one obtained immerses in mixed solution A, then transfer in reactor, be after heating 0.5h ~ 72h under the condition of 90 DEG C ~ 200 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 1mol/L and concentration the be urea liquid of 0.0001mol/L ~ 1mol/L is 1:50;
Three, be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration by concentration be stir 5min ~ 720min after the sodium molybdate solution mixing of 0.0001mol/L ~ 3mol/L, obtain mixed solution B, superficial growth step 2 obtained has the collector of cobalt oxide to immerse in mixed solution B, then transfer in reactor, be after heating 0.5h ~ 48h under the condition of 90 DEG C ~ 220 DEG C in temperature, product is taken out from reactor, product adopts water cleaning 3 ~ 5 times, adopt ethanol purge again 3 ~ 5 times, obtain the collector that superficial growth has cobalt oxide and cobalt molybdate; The volume ratio of described concentration to be the cobalt nitrate solution of 0.0001mol/L ~ 2mol/L and concentration the be sodium molybdate solution of 0.0001mol/L ~ 3mol/L is 1:60;
Four, put into water after being mixed by PVA and KOH and stir 1h ~ 96h, obtain mixed solution C; The volume ratio of described PVA and KOH is 1:(1 ~ 30);
Five, the superficial growth obtained in two panels step 3 has between cobalt oxide and the collector of cobalt molybdate and arranges the fibre resin barrier film that a layer thickness is 0.1mm, obtain the assembly of three-decker, then the assembly of three-decker is immersed in the mixed solution C that step 4 obtains, soaking 1min ~ 120min, is then dry 1h ~ 72h in the baking oven of 40 DEG C ~ 120 DEG C in temperature; Then metal shell on it is outside coated, obtains the miniature memory device of the portable clean energy.
2. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that being placed in the dilute hydrochloric acid solution ultrasonic cleaning 40min that concentration is 0.08mol/L in step one.
3. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that under temperature is the condition of 100 DEG C, heating 1h in step 2.
4. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that under temperature is the condition of 110 DEG C, heating 2h in step 2.
5. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that under temperature is the condition of 100 DEG C, heating 0.8h in step 3.
6. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that the volume ratio of PVA and KOH described in step 4 is 1:3.
7. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, is characterized in that the volume ratio of PVA and KOH described in step 4 is 1:8.
8. the preparation method of the miniature memory device of a kind of portable clean energy according to claim 1, to is characterized in that in step 5 in temperature being dry 24h in the baking oven of 60 DEG C.
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CN104495956A (en) * 2014-12-10 2015-04-08 北京化工大学 Preparation method of controllable-shape tricobalt tetraoxide by changing anions
CN104609479A (en) * 2015-02-11 2015-05-13 天津理工大学 Method for preparing Co3O4 nanoribbon
CN104752071A (en) * 2015-04-01 2015-07-01 安徽师范大学 Cobaltosic oxide and cobalt molybdate core-shell heterostructure nanowire array, preparation method and application thereof

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