CN105648422A - Gaseous phase atomic layer deposition device for electrode powder material coating and application - Google Patents
Gaseous phase atomic layer deposition device for electrode powder material coating and application Download PDFInfo
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- CN105648422A CN105648422A CN201610025327.3A CN201610025327A CN105648422A CN 105648422 A CN105648422 A CN 105648422A CN 201610025327 A CN201610025327 A CN 201610025327A CN 105648422 A CN105648422 A CN 105648422A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45523—Pulsed gas flow or change of composition over time
- C23C16/45525—Atomic layer deposition [ALD]
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a gaseous phase atomic layer deposition device for electrode powder material coating and a method for electrode powder material coating. The gaseous phase atomic layer deposition device comprises a vacuum reaction cavity and a monitoring system. A stirring device is arranged in the vacuum reaction cavity. The stirring device is in electric connection or in signal connection with the monitoring system and is controlled to operate through the monitoring system. According to the gaseous phase atomic layer deposition device, the stirring device is added in the reaction cavity, an electrode powder material is fully dispersed through the stirring device, aggregation of the electrode powder material is reduced, precursor adsorption and reaction are facilitated, the coating uniformity and efficiency are improved, and a foundation for mass production of the high-quality battery electrode powder coating material is laid.
Description
Technical field
The application relates to the electrode material manufacture field of lithium ion battery, particularly relates to gas phase apparatus for atomic layer deposition and application thereof that a kind of electrode powder body material for lithium ion battery is coated with.
Background technology
Lithium ion battery is had the excellent performances such as height ratio capacity, high cycle performance, high-energy-density and high power density because of it, has been widely used for small-sized movable digital electronic goods, including mobile phone, camera, notebook computer etc. Along with the fast development of lithium ion battery technology, lithium ion battery is also acknowledged as most promising electric powered motor energy-storage battery. The electrode powder body material of lithium ion battery, its performance decides the performance of lithium ion battery to a great extent. Research display, by being effectively improved the performance of lithium ion battery in electrode powder body material coating modification.
The electrode powder body material method for coating of existing lithium ion battery mainly has solid phase method, liquid phase method and vapor phase method. Wherein, technique for atomic layer deposition is a kind of special chemical vapour deposition technique, and the rete of preparation has the advantages such as uniform, fine and close, thickness controllable precise, high conformality. Utilize technique for atomic layer deposition to carry out electrode powder body material cladding, refer at electrode powder body material surface by from limiting Chemisorption, obtaining the rete of nanometer grade thickness one layer highly uniform.
But, the electrode powder body material of lithium ion battery has bigger specific surface area and higher specific surface energy, this causes serious particle agglomeration phenomenon, the uniformity of impact cladding and efficiency, and then affects the performance of coating modification electrode powder body material and the performance of lithium ion battery. This is particularly acute when a large amount of powder body carrying out industrialized production are coated with; Seriously constrain development further and the large-scale industrialization application of lithium ion cell electrode powder body material coating modification. Therefore, it is necessary to traditional device that substrate surface carries out ald is improved, to meet the Production requirement of this special powder material coating modification of lithium ion cell electrode powder body material.
Summary of the invention
The purpose of the application is to provide gas phase apparatus for atomic layer deposition and the application thereof of the electrode powder body material cladding being used in particular for lithium ion battery of a kind of improvement.
The application have employed techniques below scheme:
The one side of the application discloses a kind of gas phase apparatus for atomic layer deposition for electrode powder body material cladding, including vacuum response cavity and monitoring system, vacuum response cavity is provided with agitating device, agitating device is connected with monitoring system electrical connection or signal, controls agitating device operation by monitoring system.
The gas phase apparatus for atomic layer deposition of the application, is a kind of device realizing gas-solid alternation response, concrete, being put into solid particle in reaction cavity, then pass to vaporous precursors, vaporous precursors contacts with solid particle, adsorb in solid particles surface, react, form the device of clad. Because vaporous precursors is molecule or atomic form carries out adsorbing, reacting in solid particles surface, with monatomic form membrane in layer be coated on solid particles surface, so being called gas phase ald.
It should be noted that, the application it is critical only that, based on existing gas phase apparatus for atomic layer deposition, its vacuum response cavity arranges agitating device, utilize agitating device by fully dispersed for electrode powder body material, reduce electrode powder body material and reunite, be beneficial to presoma absorption and reaction, so that gas phase ald is evenly, produce high-quality electrode-clad material; Further, the gas phase apparatus for atomic layer deposition of the application is particularly suitable for the process of high-volume electrode powder body material, it is possible to meet the demand of industrialization large-scale production. Additionally, agitating device is with the connection of monitoring system, it is primarily to and is easy to monitor in real time and controls the velocity of rotation of agitating device. The application it is critical only that increase agitating device, as other, such as vacuum system, presoma system, heating system, and monitoring system etc., with reference to existing gas phase apparatus for atomic layer deposition, tired can state at this.
Therefore, in a kind of implementation of the application, gas phase apparatus for atomic layer deposition also includes vacuum system, presoma system and heating system; Vacuum system is for vacuum response cavity evacuation, presoma system is for providing presoma to vacuum response cavity, heating system is for heating to vacuum response cavity, monitoring system is for detecting the pressure and temperature in vacuum reaction chamber body, and controls being turned on and off of vacuum system, presoma system and heating system.
Preferably, agitating device is at least one in paddle stirring, turbine type stirring and frame type stirring.
It should be noted that the agitating device of the application, electrode powder body material is kicked up by its purpose exactly so that it is fully dispersed, in order to presoma absorption and reaction; Therefore, as long as electrode powder body material can be kicked up, as for adopting what kind of concrete structure can determine according to different working conditions, the preferred version of the application adopt at least one in paddle stirring, turbine type stirring and frame type stirring realize agitating function. It is appreciated that, working condition allow or some in particular cases, even can adopt structure and mode that similar washing machine drum rotates, electrode powder body material is made to kick up, such as vacuum response cavity own rotation, in this case, vacuum response cavity self structure is equivalent to the agitating device of the application.
Preferably, vacuum response cavity is made up of upper cavity and lower chamber, and one end of agitating device is fixed on upper cavity top, and the other end stretches in lower chamber.
The another side of the application discloses the application in the Surface coating of powder body material of the gas phase apparatus for atomic layer deposition of the application.
It should be noted that, although the gas phase apparatus for atomic layer deposition of the application is the cladding for electrode powder body material and designs, but, the gas phase apparatus for atomic layer deposition of the application also not only limits the use of in the cladding of electrode powder body material, and the granule of any needs cladding can adopt the gas phase apparatus for atomic layer deposition of the application.
The another side of the application discloses the method for a kind of electrode powder body material cladding, wherein, electrode powder body material is lithium ion cell positive powder body material or lithium ion battery negative powder body material, and the method adopts the gas phase apparatus for atomic layer deposition of the application that electrode powder body material is carried out coating modification.
In a kind of specific implementation of the application, the method comprises the following steps,
A pending electrode powder body material is loaded the vacuum response cavity of gas phase apparatus for atomic layer deposition by ();
B vacuum response cavity is carried out evacuation by (), maintain vacuum response cavity being effectively isolated with outside atmosphere;
C () utilizes agitating device to be kicked up by electrode powder body material so that it is fully dispersed;
D () passes into the first vaporous precursors in vacuum response cavity so that it is be adsorbed on electrode powder body material surface;
E () passes into carrier gas and is removed by the first vaporous precursors unnecessary in vacuum response cavity;
F () passes into the second vaporous precursors in vacuum response cavity, so as to react with the first vaporous precursors being adsorbed on electrode powder body material surface, form clad;
G () passes into carrier gas and is removed by the second vaporous precursors unnecessary in vacuum response cavity;
Repeat step (d) to (g) until obtaining the clad setting thickness or structure.
It should be noted that, step (d) to (g) actually can complete one layer of gas phase ald cladding, but, in order to obtain thicker clad, typically require and carry out Multiple depositions, accordingly, it would be desirable to repeat step (d) to (g) until obtaining the clad of desired thickness; As for specifically needing to repeat how many times, depend on the first the concrete vaporous precursors and the second vaporous precursors that adopt and concrete required coating thickness, be not specifically limited at this.
It can further be stated that, adopt the gas phase apparatus for atomic layer deposition of the application and method electrode powder body material can be carried out one, two kinds, the even cladding of multiple material, forms the clad of different structure, as long as changing the first vaporous precursors corresponding and the second vaporous precursors. Additionally, the first vaporous precursors and the second vaporous precursors, being actually it is assumed that two kinds of presoma reactions can obtain clad, this is to obtain clad than more conventional reaction pattern, therefore so assumes.
It is appreciated that, if the first vaporous precursors is adsorbed on electrode powder body material surface, it is then passed through some specific conditions and just can form clad, certainly avoid the need for passing into the second vaporous precursors again, namely can omit step (f) and (g). Or, if needing more kinds of vaporous precursors could react generation clad, such as also need to the third vaporous precursors, the 4th kind of vaporous precursors, even when more presoma, accordingly increase and pass into vaporous precursors, unnecessary vaporous precursors is cleaned in carrier gas, pass into another kind of vaporous precursors again, carry out carrier gas cleaning again, so repeatedly.
Preferably, the mixing speed of agitating device is 100-1000 rpm.
It should be noted that mixing speed is the difference of the electrode powder body material granule initial size according to lithium ion battery and quality and regulates; Rotating speed is too low, and the electrode powder body material of accumulation cannot be fully dispersed, and rotating speed is too high, and electrode powder body material granule, due to the effect of centrifugal force, can be drawn close to reaction chamber body wall, run counter to the scattered original intention of electrode powder body material. For this, confirm through substantial amounts of test, for the electrode powder body material of the big micron particles of initial size and quality, regulate mixing speed 500-1000 rpm, it is possible to reach comparatively ideal powder body dispersion effect; And the electrode powder body material to the little nano-scale particle of initial size and quality, regulate mixing speed 100-500 rpm, it is possible to reach comparatively ideal powder body dispersion effect.
Preferably, in vacuum response cavity, the reaction temperature of the first vaporous precursors and the second vaporous precursors is 50-300 DEG C.
It should be noted that the first vaporous precursors and the reaction temperature of the second vaporous precursors, being actually the temperature in vacuum reaction chamber body, this is to be controlled heating system by monitoring system to be heated so that it is be maintained at temperature required; Wherein, concrete reaction temperature is fixed according to the concrete presoma adopted and required reaction temperature thereof, is not specifically limited at this; As a rule, according to the cladding material that electrode powder body material adopts, reaction temperature is all between 50-300 DEG C.
Preferably, carrier gas is noble gas. It is furthermore preferred that carrier gas is nitrogen or argon.
Preferably, the temperature of carrier gas is 50-300 DEG C.
It should be noted that the one of carrier gas is mainly used for cleaning up the first vaporous precursors and the second vaporous precursors, but, in order to avoid the temperature in vacuum reaction chamber body is impacted, therefore, adopting temperature is the carrier gas of 50-300 DEG C; It is appreciated that concrete carrier gas temperature is consistent with the reaction temperature in vacuum response cavity, is not specifically limited at this.
Preferably, the temperature of the first vaporous precursors and the second vaporous precursors is 50-200 DEG C.
It should be noted that the fusing point of presoma is more high, its saturated vapor pressure is more low, and the forerunner's scale of construction that can participate in reaction obtained under equal conditions is more few; Therefore, for common precursor, temperature controls at 50-100 degree Celsius; For the solid precursor that fusing point is significantly high, temperature can reach 200 degrees Celsius. It is appreciated that the condensation in order to prevent presoma in transfer pipeline, therefore, it is also desirable to pipeline is heated so that it is temperature controls at 50-200 degree Celsius.
The application has the beneficial effects that:
The gas phase apparatus for atomic layer deposition of the application, design particular for the coating modification of lithium ion cell electrode powder body, agitating device is increased in reaction cavity, utilize the electrode powder body material of agitating device stirring lithium ion battery, and, by regulating rotating speed and the direction of agitating device, the electrode powder body material making different quality and particle diameter obtains fully dispersed, effectively reduce the reunion degree of powder body, it is beneficial to absorption and the reaction of presoma, improve being evenly coated property and coating efficiency, lay a good foundation for the high-quality lithium ion cell electrode powder body cladding material of industrialization large-scale production.
Accompanying drawing explanation
Fig. 1 is the structural representation of gas phase apparatus for atomic layer deposition in the embodiment of the present application;
Fig. 2 is the schematic process flow diagram of electrode powder body material method for coating in the embodiment of the present application;
Fig. 3 is the transmission electron microscope figure in the embodiment of the present application before and after electrode powder body material cladding, and (a) is the scanning result before cladding, and (b) is the scanning result after cladding.
Detailed description of the invention
The gas phase apparatus for atomic layer deposition of the application, improve particular for the cladding of lithium ion cell electrode powder body material, concrete, vacuum response cavity arranges agitating device, agitating device is utilized to be kicked up by electrode powder body material, it is made to disperse, thus being beneficial to presoma to be adsorbed on electrode powder body material particle surface uniformly and effectively so that gas phase ald is coated with evenly.
It is appreciated that, the gas phase apparatus for atomic layer deposition for electrode powder body material cladding of the application, although improving particular for the cladding of lithium ion cell electrode powder body material, but, this gas phase apparatus for atomic layer deposition also not only limits the use of in the cladding of lithium ion cell electrode powder body material, it is also possible to form the situation of one layer of clad at particle surface for other various needs.
It should be noted that the method for the electrode powder body material cladding of the application, it it is the situation of the commonplace two kind presoma reaction formation clad adopted; The gas phase apparatus for atomic layer deposition of the application or method for coating, it is not only limited in two kinds of presomas, can also adopt three kinds or more kinds of presoma realizes the preparation of multi-layer film structure according to a definite sequence, corresponding in method for coating, after the second vaporous precursors cleans, pass into the third vaporous precursors, then adopt carrier gas to clean the third vaporous precursors, pass into the 4th kind of vaporous precursors, carrier gas is cleaned, by that analogy.
Additionally, after passing into presoma, it is possible to adopt pressurize absorption or not pressurize absorption, pressurize is adsorbed namely when passing into presoma, closes vacuum system, allows the air pressure keeping certain in vacuum reaction chamber body, so that presoma absorption, it is then turned on vacuum system after a period of time, presoma is detached; Not pressurize is adsorbed, then be when passing into presoma, opens vacuum system, makes the air pressure in vacuum reaction chamber body remain at initial gas pressure. Concrete employing pressurize absorption still not pressurize absorption, it is possible to determine according to the absorption complexity of each presoma, be not specifically limited at this.
Below by specific embodiment, the application is described in further detail. The application is only further described by following example, should not be construed as the restriction to the application.
Embodiment
The gas phase apparatus for atomic layer deposition for electrode powder body material cladding of this example, by vacuum response cavity, vacuum system, presoma system, heating system, and monitoring system composition. Wherein, presoma system for inputting carrier gas and vaporous precursors to vacuum response cavity. Heating system is for heating vacuum response cavity, precursor container and connecting line. Vacuum system is for maintaining the discharge of remaining presoma, by-product etc. in the vacuum of vacuum response cavity, the internal pressure adjusting vacuum response cavity and vacuum reaction chamber body. Monitoring system is for monitoring and show the temperature of the pressure of vacuum response inside cavity, conversion zone, the external wall temperature of vacuum reaction chamber, precursor container temperature, connecting line temperature etc.; And control presoma burst length and flow, cycle-index and carrier gas scavenging period and flow in presoma system, control the switch of heating system and vacuum system.
In this example, vacuum response cavity is as shown in Figure 1, whole vacuum response cavity relies on bracing frame 15, vacuum response cavity is made up of lower chamber 1 and upper cavity 2, lower chamber 1 is fixed on bracing frame 15, upper cavity 2 is connected on bracing frame 15 by guide rail wheel 14, and upper cavity 2 can be moved up and down along bracing frame 15 by guide rail wheel 14;One end of agitating device 4 is fixed on upper cavity 2 top, is sealed by sealing member 3, and when upper cavity 2 and lower chamber 1 close up, agitating device 4 other end stretches in lower chamber 1. It addition, vacuum response cavity is further opened with feeding port 5, air inlet 6, gas outlet 7, lower chamber hot oil inlet 8, lower chamber hot oil outlet 9, upper cavity hot oil inlet 10 and upper cavity hot oil outlet 11.
Wherein, feeding port 5 is arranged at the top of upper cavity 2, is used for adding electrode body material. Air inlet 6 is opened in the bottom of lower chamber 1, is used for connecting presoma system; In this example, presoma system includes two presoma in parallel conveying branch roads, provides the first vaporous precursors and the precursor material of the second vaporous precursors respectively, and precursor material passes into vacuum response cavity by air inlet 6. Gas outlet is opened in the top of upper cavity 2, it is positioned at feeding port 5 side, for connecting vacuum system, vacuum response cavity is bled by the vacuum pump 13 of vacuum system by gas outlet 7, to maintain the vacuum of vacuum response cavity, to adjust the discharge etc. of remaining presoma and/or by-product in vacuum response inside cavity pressure and vacuum reaction chamber body; Further, in a kind of implementation of the application, between vacuum pump 13 and gas outlet 7, dust filtering device 12 it is additionally provided with, for a small amount of dust that filtration residue presoma and/or by-product and carrier gas are taken out of from reaction cavity. Lower chamber hot oil inlet 8 and lower chamber hot oil outlet 9 are opened on lower chamber 1, lower chamber hot oil inlet 8 is opened in the lower side of lower chamber 1, lower chamber hot oil outlet 9 is opened in the upper side of lower chamber 1, for connecting heating system, deep fat after heating enters through lower chamber hot oil inlet 8, is then discharged by lower chamber hot oil outlet 9, in this process, transfer heat to lower chamber 1, to realize lower chamber 1 is heated. Similar, it is opened in upper cavity hot oil inlet 10 and the upper cavity hot oil outlet 11 of upper cavity 2, is also used for connecting heating system, by deep fat, upper cavity 2 is heated.
Adopt the method that electrode powder body material is coated with by the gas phase apparatus for atomic layer deposition of this example, as in figure 2 it is shown, comprise the following steps:
A pending electrode powder body material is loaded the vacuum response cavity of gas phase apparatus for atomic layer deposition by ();
B () is opened vacuum system and vacuum response cavity is carried out evacuation, maintain vacuum response cavity being effectively isolated with outside atmosphere;
C () opens agitating device, utilize agitating device to be kicked up by electrode powder body material, make electrode powder body material fully dispersed;
D () passes into the first vaporous precursors in vacuum response cavity, make the first vaporous precursors be adsorbed on electrode powder body material surface; Burst length is the 1-10 second, it is preferred to the 1-5 second;
E () passes into carrier gas and cleans the first vaporous precursors excessive in reaction cavity, be namely removed without being adsorbed on the first vaporous precursors of electrode powder body material particle surface; In the process cleaned, being not usually required to stopping stirring, equipped with the drainage screen that aperture is only small on bleeding point, therefore, electrode powder body will not be pumped;
F () passes into the second vaporous precursors in vacuum response cavity, the burst length is the 1-10 second, it is preferred to the 1-5 second, makes the second vaporous precursors and the first vaporous precursors being adsorbed on electrode powder body material surface reacts, and forms monoatomic layer rete;
G () passes into carrier gas and cleans the second vaporous precursors excessive in reaction cavity, be namely removed without participating in the second vaporous precursors of reaction and by-product that the first vaporous precursors reacts with the second vaporous precursors;
Repeat step (d) to (g) until obtaining the clad setting thickness.
Wherein, in step (d) or (f), different with quality according to the granular size of pending electrode powder body material, regulate the rotating speed of agitating device. Concrete, for the micron particles that initial size and quality are big, regulate agitating device rotating speed and be 500-1000 rpm, it is possible to electrode powder body material is effectively disperseed; The nano-scale particle that initial size and quality is little, regulates agitating device rotating speed and is 100-500 rpm, it is possible to effectively disperseed by electrode powder body material.
Burst length for the first vaporous precursors and the second vaporous precursors, owing to deposition process needs certain time to make presoma be adsorbed on particle surface completely, if the burst length was less than 1 second, then to pass into forerunner's scale of construction of offer very few for single, it is impossible to the electrode powder body material granule that effectively cladding is fully dispersed; And the presoma burst length was more than 5 seconds, the presoma passed into is taken away by vacuum pump, causes the waste of presoma; Therefore, the presoma burst length is the 1-10 second, it is preferred to the 1-5 second.
In step (d) or (f), concrete, according to the complexity that different lithium ion battery powder particle surface is adsorbed by different presomas, what regulate presoma pulse passes into number of times, being advisable with 10-20 time, pass into number of times very little, the ratio of absorption is not high; Passing into number of times too many, what pass into number of times increases the contribution for presoma absorption not quite, and presoma is taken away by vacuum pump, causes the waste of presoma. In this example, presoma pulse refers to, for instance passes into the first presoma 5 seconds, then turns off and pass into, then passes into 5 seconds, stops, passing into 5s, 10 times so repeatedly. It should be noted that owing to presoma is contained in precursor container, and there is certain saturated vapor pressure; Pass into 5 seconds, stop; Treat that in precursor container, pressure returns to saturated vapor pressure, then pass into 5 seconds; So can increase the loading of presoma; Each 5 seconds, 10 subpulses, more much bigger than single passes into 50 seconds loading. It addition, the time suspended is generally at about 2 seconds. In the process passing into presoma, if pressurize, then closing vacuum pump, vacuum pump is then opened in not pressurize; Concrete employing pressurize absorption still not pressurize absorption, it is possible to determine according to the absorption complexity of each presoma.
The wall body of vacuum response cavity is heated by the heating system of this example, inside by the heat radiation heating vacuum response cavity of wall body, electrode powder body material granule therein is made to reach the temperature needed for reaction condition, this reaction condition, the i.e. reaction temperature of the first vaporous precursors and the second vaporous precursors, generally this temperature is between 50-300 degree Celsius, and concrete reaction temperature is determined according to the first concrete vaporous precursors and the second vaporous precursors.
It addition, for the presoma itself passing into vacuum response cavity, its temperature controls at 25-200 degree Celsius. The fusing point of presoma is more high, and its saturated vapor pressure is more low, and the forerunner's scale of construction that can participate in reaction obtained under equal conditions is more few. For common precursor, temperature controls at 25-100 degree Celsius; For the solid precursor that fusing point is significantly high, temperature can reach 200 degrees Celsius. The temperature of presoma pipeline controls at 25-200 degree Celsius, it is prevented that presoma condensation in transfer pipeline.
In the application, presoma can be gaseous state, liquid, solid-state or plasma state. Vacuum response cavity is brought in liquid or the available carrier gas of solid precursor into, then cleans with pure carrier gas; Gaseous state or plasma state presoma can utilize carrier gas to bring reaction cavity into, it is also possible to be passed directly into vacuum response cavity.
The carrier gas of this example is noble gas, it is preferred to nitrogen.The temperature of carrier gas is 50-300 degree Celsius, and in general, the temperature of carrier gas is suitable with the reaction temperature in vacuum reaction chamber body, to reduce the impact on vacuum response inside cavity conversion zone temperature homogeneity.
Test 1
Lithium ion battery powder material, using trimethyl aluminium (abbreviation TMA) and water as the first presoma and the second presoma, according to the step shown in previously described Fig. 2, is carried out coating modification by this test, concrete:
The first step: the lithium ion battery powder material that reaction cavity loads is LiNiMnCoO2Tertiary cathode material, the particle diameter of positive electrode is about 10 microns.
Second step: reaction cavity evacuation, maintains reaction cavity being effectively isolated outside atmosphere. Wherein, vacuum reaches 100-300mTorr, and that this example is concrete is 200mTorr.
3rd step: opening agitating device, the rotating speed of agitating device is 500 rpms, makes the lithium ion battery powder material of different quality and particle diameter obtain fully dispersed.
4th step: the first vaporous precursors trimethyl aluminium TMA is by carrier gas N2Auxiliary passes into reaction cavity, burst length is 1 second, TMA physical absorption is on the surface of lithium ion battery powder granule, pass into TMA presoma 10 times, reaction cavity is not bled by this process, it is provided that the dwell time of the elevated pressures of 100-300 second, the concrete pressurize of this example 200 seconds, increase the time of contact of presoma TMA and powder granule surface, to improve being evenly coated property and coating efficiency.
5th step: pass into carrier gas N2Clean the first vaporous precursors excessive in reaction cavity, be removed without being adsorbed on the first vaporous precursors of lithium ion battery powder particle surface, flushing times 30 seconds.
6th step: the second vaporous precursors water, identical with the method that the 4th step deposits TMA, by carrier gas nitrogen auxiliary, steam is passed into reaction cavity, same pressurize 200 seconds, water is adsorbed on the presoma TMA of lithium ion battery powder particle surface and front surface absorption with it and chemical reaction occurs, and generates the rete of monoatomic layer.
7th step: identical with the cleaning method of the 5th step, removes and fails the presoma water that reacts with presoma TMA and by-product that presoma TMA reacts with presoma water. Because the viscosity of water is higher, can proper extension scavenging period, the prolongation scavenging period that this example is concrete is 2 minutes.
8th step: according to required coating modification layer thickness, repeats the 4th step to the 7th step, can be accurately obtained the coating modification layer of desired thickness. This example is specifically repeated 10 times, finally prepares the coating modification layer that thickness is about 3 nanometers.
Utilize the pattern of granule before and after transmission electron microscope tem observation cladding, as shown in Figure 3. In Fig. 3, (a) is the scanning result before cladding, and (b) is the scanning result after cladding, it can be seen that clad is high-visible, and thickness is uniform, and has high shape-retaining ability.
Test 2
Lithium ion battery powder material, using diethyl zinc (abbreviation DEZ) and water as the first presoma and the second presoma, according to the step shown in previously described Fig. 2, is carried out coating modification by this test, concrete:
The first step: the lithium ion battery powder material that reaction cavity loads is LiNiMnCoO2Tertiary cathode material, the particle diameter of positive electrode is about 10 microns.
Second step: reaction cavity evacuation, maintains reaction cavity being effectively isolated outside atmosphere. Wherein, vacuum reaches 100-300mTorr, and that this example is concrete is 200mTorr.
3rd step: opening agitating device, the rotating speed of agitating device is 500 rpms, makes the lithium ion battery powder material of different quality and particle diameter obtain fully dispersed.
4th step: the first vaporous precursors diethyl zinc DEZ is by carrier gas N2Auxiliary passes into reaction cavity, burst length is 1 second, DEZ physical absorption is on the surface of lithium ion battery powder granule, pass into DEZ presoma 10 times, reaction cavity is not bled by this process, it is provided that the dwell time of the elevated pressures of 100-300 second, the concrete pressurize of this example 200 seconds, increase the time of contact of presoma DEZ and powder granule surface, to improve being evenly coated property and coating efficiency.
5th step: pass into carrier gas N2Clean the first vaporous precursors excessive in reaction cavity, be removed without being adsorbed on the first vaporous precursors of lithium ion battery powder particle surface, flushing times 30 seconds.
6th step: the second vaporous precursors water H2O, identical with the method that the 4th step deposits DEZ, same pressurize 200 seconds, water is adsorbed on the presoma DEZ of lithium ion battery powder particle surface and front surface absorption with it and chemical reaction occurs, and generates the rete of monoatomic layer.
7th step: identical with the cleaning method of the 5th step, removes and fails the presoma water that reacts with presoma DEZ and by-product that presoma DEZ reacts with presoma water. Because the viscosity of water is higher, can proper extension scavenging period, the prolongation scavenging period that this example is concrete is 2 minutes.
8th step: according to required coating modification layer thickness, repeats the 4th step to the 7th step, can be accurately obtained the coating modification layer of desired thickness. This example is specifically repeated 10 times, finally prepares the coating modification layer that thickness is about 3 nanometers.
Utilize the pattern of granule before and after transmission electron microscope tem observation cladding, it can be seen that clad is high-visible, and thickness is uniform, and being evenly coated property is good, has high shape-retaining ability; Further, even particle size before and after cladding, almost without agglomeration.
Test 3
Lithium ion battery powder material, using four (dimethylamino) titanium (abbreviation TDMAT) and water as the first presoma and the second presoma, according to the step shown in previously described Fig. 2, is carried out coating modification by this test, concrete:
The first step: the lithium ion battery powder material that reaction cavity loads is LiNiMnCoO2Tertiary cathode material, the particle diameter of positive electrode is about 10 microns.
Second step: reaction cavity evacuation, maintains reaction cavity being effectively isolated outside atmosphere. Wherein, vacuum reaches 100-300mTorr, and that this example is concrete is 200mTorr.
3rd step: opening agitating device, the rotating speed of agitating device is 500 rpms, makes the lithium ion battery powder material of different quality and particle diameter obtain fully dispersed.
4th step: the first vaporous precursors four (dimethylamino) titanium TDMAT is by carrier gas N2Auxiliary passes into reaction cavity, burst length is 1 second, TDMAT physical absorption is on the surface of lithium ion battery powder granule, pass into TDMAT presoma 10 times, reaction cavity is not bled by this process, it is provided that the dwell time of the elevated pressures of 100-300 second, the concrete pressurize of this example 200 seconds, increase the time of contact of presoma TDMAT and powder granule surface, to improve being evenly coated property and coating efficiency.
5th step: pass into carrier gas N2Clean the first vaporous precursors excessive in reaction cavity, be removed without being adsorbed on the first vaporous precursors of lithium ion battery powder particle surface, flushing times 30 seconds.
6th step: the second vaporous precursors water H2O, identical with the method that the 4th step deposits TDMAT, same pressurize 200 seconds, water is adsorbed on the presoma TDMAT of lithium ion battery powder particle surface and front surface absorption with it and chemical reaction occurs, and generates the rete of monoatomic layer.
7th step: identical with the cleaning method of the 5th step, removes and fails the presoma water that reacts with presoma TDMAT and by-product that presoma TDMAT reacts with presoma water. Because the viscosity of water is higher, can proper extension scavenging period, the prolongation scavenging period that this example is concrete is 2 minutes.
8th step: according to required coating modification layer thickness, repeats the 4th step to the 7th step, can be accurately obtained the coating modification layer of desired thickness. This example is specifically repeated 60 times, finally prepares the coating modification layer that thickness is about 3 nanometers.
Utilize the pattern of granule before and after transmission electron microscope tem observation cladding, it can be seen that clad is high-visible, and thickness is uniform, and being evenly coated property is good, has high shape-retaining ability; Further, even particle size before and after cladding, almost without agglomeration.
Test 4
This test is using three (diethylamino) t-butyl carboxamide tantalum (abbreviation TBTDET) and water as the first presoma and the second presoma, according to the step shown in previously described Fig. 2, lithium ion battery powder material is carried out coating modification, concrete:
The first step: the lithium ion battery powder material that reaction cavity loads is LiNiMnCoO2Tertiary cathode material, the particle diameter of positive electrode is about 10 microns.
Second step: reaction cavity evacuation, maintains reaction cavity being effectively isolated outside atmosphere. Wherein, vacuum reaches 100-300mTorr, and that this example is concrete is 200mTorr.
3rd step: opening agitating device, the rotating speed of agitating device is 500 rpms, makes the lithium ion battery powder material of different quality and particle diameter obtain fully dispersed.
4th step: the first vaporous precursors three (diethylamino) t-butyl carboxamide tantalum TBTDET is by carrier gas N2Auxiliary passes into reaction cavity, burst length is 1 second, TBTDET physical absorption is on the surface of lithium ion battery powder granule, pass into TBTDET presoma 10 times, reaction cavity is not bled by this process, it is provided that the dwell time of the elevated pressures of 100-300 second, the concrete pressurize of this example 200 seconds, increase the time of contact of presoma TBTDET and powder granule surface, to improve being evenly coated property and coating efficiency.
5th step: pass into carrier gas N2Clean the first vaporous precursors excessive in reaction cavity, be removed without being adsorbed on the first vaporous precursors of lithium ion battery powder particle surface, flushing times 30 seconds.
6th step: the second vaporous precursors water H2O, identical with the method that the 4th step deposits TBTDET, same pressurize 200 seconds, water is adsorbed on the presoma TBTDET of lithium ion battery powder particle surface and front surface absorption with it and chemical reaction occurs, and generates the rete of monoatomic layer.
7th step: identical with the cleaning method of the 5th step, removes and fails the presoma water that reacts with presoma TBTDET and by-product that presoma TBTDET reacts with presoma water. Because the viscosity of water is higher, can proper extension scavenging period, the prolongation scavenging period that this example is concrete is 2 minutes.
8th step: according to required coating modification layer thickness, repeats the 4th step to the 7th step, can be accurately obtained the coating modification layer of desired thickness. This example is specifically repeated 10 times, finally prepares the coating modification layer that thickness is about 1 nanometer.
Utilize the pattern of granule before and after transmission electron microscope tem observation cladding, it can be seen that clad is high-visible, and thickness is uniform, and being evenly coated property is good, has high shape-retaining ability; Further, even particle size before and after cladding, almost without agglomeration.
Test 5
This test is using four (ethyl-methyl amido) hafnium (abbreviation TEMAH) and water as the first presoma and the second presoma, according to the step shown in previously described Fig. 2, lithium ion battery powder material is carried out coating modification, concrete:
The first step: the lithium ion battery powder material that reaction cavity loads is LiNiMnCoO2Tertiary cathode material, the particle diameter of positive electrode is about 10 microns.
Second step: reaction cavity evacuation, maintains reaction cavity being effectively isolated outside atmosphere. Wherein, vacuum reaches 100-300mTorr, and that this example is concrete is 200mTorr.
3rd step: opening agitating device, the rotating speed of agitating device is 500 rpms, makes the lithium ion battery powder material of different quality and particle diameter obtain fully dispersed.
4th step: the first vaporous precursors four (ethyl-methyl amido) hafnium TEMAH is by carrier gas N2Auxiliary passes into reaction cavity, burst length is 1 second, TEMAH physical absorption is on the surface of lithium ion battery powder granule, pass into TEMAH presoma 10 times, reaction cavity is not bled by this process, it is provided that the dwell time of the elevated pressures of 100-300 second, the concrete pressurize of this example 200 seconds, increase the time of contact of presoma TEMAH and powder granule surface, to improve being evenly coated property and coating efficiency.
5th step: pass into carrier gas N2Clean the first vaporous precursors excessive in reaction cavity, be removed without being adsorbed on the first vaporous precursors of lithium ion battery powder particle surface, flushing times 30 seconds.
6th step: the second vaporous precursors water H2O, identical with the method that the 4th step deposits TEMAH, same pressurize 200 seconds, water is adsorbed on the presoma TEMAH of lithium ion battery powder particle surface and front surface absorption with it and chemical reaction occurs, and generates the rete of monoatomic layer.
7th step: identical with the cleaning method of the 5th step, removes and fails the presoma water that reacts with presoma TEMAH and by-product that presoma TEMAH reacts with presoma water. Because the viscosity of water is higher, can proper extension scavenging period, the prolongation scavenging period that this example is concrete is 2 minutes.
8th step: according to required coating modification layer thickness, repeats the 4th step to the 7th step, can be accurately obtained the coating modification layer of desired thickness. This example is specifically repeated 50 times, finally prepares the coating modification layer that thickness is about 3 nanometers.
Utilize the pattern of granule before and after transmission electron microscope tem observation cladding, it can be seen that clad is high-visible, and thickness is uniform, and being evenly coated property is good, has high shape-retaining ability; Further, even particle size before and after cladding, almost without agglomeration.
The gas phase apparatus for atomic layer deposition for lithium ion cell electrode powder body material coating modification of this example is by introducing agitating device, the independent rotating speed regulating agitating device realizes the fully dispersed of the lithium ion cell electrode powder body material of different-grain diameter and quality, effectively alleviate the reunion degree of powder body, it is beneficial to absorption and the reaction of presoma, improve being evenly coated property and coating efficiency, it is adaptable to extensive high-quality deposition.
Above content is further description the application made in conjunction with specific embodiment, it is impossible to assert the application be embodied as be confined to these explanations.For the application person of an ordinary skill in the technical field, under the premise conceived without departing from the application, it is also possible to make some simple deduction or replace, all should be considered as belonging to the protection domain of the application.
Claims (10)
1. the gas phase apparatus for atomic layer deposition for electrode powder body material cladding, including vacuum response cavity and monitoring system, it is characterized in that: described vacuum response cavity is provided with agitating device, described agitating device is connected with the electrical connection of described monitoring system or signal, controls agitating device by described monitoring system and runs.
2. gas phase apparatus for atomic layer deposition according to claim 1, it is characterised in that: also include vacuum system, presoma system and heating system; Described vacuum system is for vacuum response cavity evacuation, described presoma system is for providing presoma to vacuum response cavity, described heating system is for heating to vacuum response cavity, described monitoring system is for detecting the temperature and pressure of vacuum reaction chamber inside and outside, and controls being turned on and off of vacuum system, presoma system and heating system.
3. gas phase apparatus for atomic layer deposition according to claim 1, it is characterised in that: described agitating device is at least one in paddle stirring, turbine type stirring and frame type stirring.
4. the gas phase apparatus for atomic layer deposition according to any one of claim 1-3, it is characterised in that: described vacuum response cavity is made up of upper cavity and lower chamber, and one end of described agitating device is fixed on upper cavity top, and the other end stretches in lower chamber.
5. the application in the Surface coating of powder body material of the gas phase apparatus for atomic layer deposition according to any one of claim 1-4.
6. the method for an electrode powder body material cladding, described electrode powder body material is lithium ion cell positive powder body material or lithium ion battery negative powder body material, it is characterised in that: described method includes adopting the gas phase apparatus for atomic layer deposition described in any one of claim 1-4 that electrode powder body material is carried out coating modification.
7. method according to claim 6, it is characterised in that: said method comprising the steps of,
A pending electrode powder body material is loaded the vacuum response cavity of described gas phase apparatus for atomic layer deposition by ();
B vacuum response cavity is carried out evacuation by ();
C () utilizes described agitating device to be kicked up by described electrode powder body material so that it is fully dispersed;
D () passes into the first vaporous precursors in vacuum response cavity so that it is be adsorbed on electrode powder body material surface;
E () passes into carrier gas and is removed by the first vaporous precursors unnecessary in vacuum response cavity;
F () passes into the second vaporous precursors in vacuum response cavity, so as to react with the first vaporous precursors being adsorbed on electrode powder body material surface, form clad;
G () passes into carrier gas and is removed by the second vaporous precursors unnecessary in vacuum response cavity;
Repeat step (d) to (g) until obtaining the clad setting thickness or structure.
8. method according to claim 7, it is characterised in that: the mixing speed of described agitating device is 100-1000 rpm.
9. method according to claim 7, it is characterised in that: in described vacuum response cavity, the reaction temperature of the first vaporous precursors and the second vaporous precursors is 50-300 DEG C.
10. method according to claim 7, it is characterised in that: the temperature of described carrier gas is 50-300 DEG C, and described carrier gas is noble gas, it is preferred that described carrier gas is argon or nitrogen.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11269647A (en) * | 1998-03-23 | 1999-10-05 | Mitsui Mining Co Ltd | Chemical vapor deposition treatment |
| CN102418085A (en) * | 2011-12-14 | 2012-04-18 | 无锡迈纳德微纳技术有限公司 | Micronano-scale powder protective layer wrapping device and method |
| CN103594684A (en) * | 2013-11-27 | 2014-02-19 | 电子科技大学 | Making method of zinc oxide or aluminum-doped zinc oxide coated lithium cobaltate electrode |
| CN104032197A (en) * | 2014-06-26 | 2014-09-10 | 武汉理工大学 | Method for preparing TiN-Ni composite ceramics |
-
2016
- 2016-01-14 CN CN201610025327.3A patent/CN105648422A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11269647A (en) * | 1998-03-23 | 1999-10-05 | Mitsui Mining Co Ltd | Chemical vapor deposition treatment |
| CN102418085A (en) * | 2011-12-14 | 2012-04-18 | 无锡迈纳德微纳技术有限公司 | Micronano-scale powder protective layer wrapping device and method |
| CN103594684A (en) * | 2013-11-27 | 2014-02-19 | 电子科技大学 | Making method of zinc oxide or aluminum-doped zinc oxide coated lithium cobaltate electrode |
| CN104032197A (en) * | 2014-06-26 | 2014-09-10 | 武汉理工大学 | Method for preparing TiN-Ni composite ceramics |
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