CN107815668B - Rotary atomic layer deposition reactor for batch modification of hollow fiber membranes - Google Patents
Rotary atomic layer deposition reactor for batch modification of hollow fiber membranes Download PDFInfo
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- CN107815668B CN107815668B CN201711265063.XA CN201711265063A CN107815668B CN 107815668 B CN107815668 B CN 107815668B CN 201711265063 A CN201711265063 A CN 201711265063A CN 107815668 B CN107815668 B CN 107815668B
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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]
- C23C16/45555—Atomic layer deposition [ALD] applied in non-semiconductor technology
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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
- C23C16/22—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 deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/40—Oxides
- C23C16/405—Oxides of refractory metals or yttrium
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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
- C23C16/458—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 supporting substrates in the reaction chamber
Abstract
The invention relates to a rotary atomic layer deposition device for batch modification of hollow fiber membranes, which is used for realizing rotation and uniform deposition of the hollow fiber membranes in a cavity. The rotary reactor comprises a cavity and an upper cover, the top of the cavity is sealed with the upper cover through a sealing ring, and the whole device can reach the vacuum degree required by experiments. The motor with the magnet is fixed on the cover of the cavity, and the magnet in the cavity rotates along with the rotation of the motor by utilizing the interaction force of the magnet. Thereby driving the porous turntable to rotate. The hollow fiber membrane is fixed on the porous turntable. The hollow fiber membrane is driven to rotate by adjusting the rotating speed of the motor, so that reactants pulsed into the cavity are uniformly diffused in the cavity and uniformly deposited on the surface of the membrane. The device of the invention accelerates the diffusion of reactants by rotating the sample, so that the whole cavity is uniformly filled with the reactants, thereby realizing the aim of depositing the modified fiber materials in a large scale and having the advantages of high efficiency, high yield and the like.
Description
Technical Field
The invention relates to an atomic layer deposition reactor, and provides a more uniform and controllable rotary atomic layer deposition reactor for modifying the surfaces of hollow fibers in batches.
Background
The polymer porous separation material plays an important role in the fields of water treatment, oil-water separation, particulate matter filtration and the like. Hollow fiber membranes offer many advantages over flat sheet membranes, such as a larger effective filtration surface area per unit volume, simple assembly manufacture, no need for feed and permeate spacers, and simpler pretreatment and maintenance. Thus, hollow fiber membranes have potential applications in the biomedical materials for chemical wastewater treatment, blood oxygenation, hemodialysis, and food processing industries. In order to achieve the desired objective, it is necessary to hydrophilically modify the properties of the surface of the polymer film material by physical or chemical means. However, the traditional method of modifying the surface of the polymer material, such as chemical modification, filling modification, blending modification or the like, needs a large amount of chemical reagents, has complicated modification process, has smaller space for improving the performance of the modified porous material, is incomplete in modification, and cannot realize precise control of the pore diameter. More importantly, the generation of large amounts of organic wastewater greatly increases the difficulty and economic cost of the subsequent treatment process.
Atomic layer deposition (atomic layer deposition, ALD) is an advanced ultra-thin film deposition technique that, due to its self-limiting nature of the reaction process, yields deposited layers with good conformality and can achieve sub-nanometer thickness control. The porous polymer separation material can be uniformly and conformally deposited in complex three-dimensional pore channels at a lower temperature, so that the porous polymer separation material becomes an important means for modifying the porous polymer separation material.
Compared with the traditional film surface modification method, the hydrophilic modified hydrophobic film surface is subjected to hydrophilic modification by atomic layer deposition oxide, so that the uniformity and the shape retention are good, the hydrophilicity is obviously increased, and the protein pollution resistance is enhanced; by changing the deposition times, the permeability and the retention rate of the hollow fiber membrane can be adjusted step by step, so that the hollow fiber membrane modified by the ALD technology has commercial application prospect.
However, most of the atomic layer deposition reactors used at present are fixed cavities, the deposition cavity is smaller, the substrate is in a standing state in the cavity, dead angles are easy to appear in the deposition reaction process, and reactant diffusion is uneven, so that film surface deposition is uneven; and the sample capacity is less, the production efficiency is lower, and the application range and the yield are limited. Therefore, development of a novel reaction chamber is needed to solve the problem that ALD is not suitable for mass deposition of fiber materials with modified high filtration area.
Disclosure of Invention
The invention provides an atomic layer deposition rotary reactor suitable for mass deposition of modified hollow fiber membranes, which can uniformly and efficiently carry out hydrophilic modification on the surfaces of the membranes and realize improvement of separation performance.
In order to achieve the above purpose, the scheme of the invention is as follows:
a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes comprises a cavity and an upper cover, wherein the top of the cavity is connected with the upper cover in a sealing way through a sealing ring, and an air inlet pipe and an air outlet pipe are arranged at the bottom of the cavity; the motor with the magnet is fixed at the top of the upper cover, and the motor drives the magnet to rotate through the rotating shaft; the same magnet is arranged in the cavity, and the magnet in the cavity rotates along with the rotation of the motor under the interaction force of the magnet; the bracket is fixed on the side wall of the cavity, and the magnet is fixed on the bracket through the rotating shaft; the end of the rotating shaft is connected with a porous rotating disc, and the hollow fiber membrane is hung on the porous rotating disc.
Wherein, the arrangement of holes in the porous turntable is concentric circle arrangement, and the hollow fiber membrane is hung on the porous turntable through a raw material belt. The sealing ring is a fluororubber O-shaped sealing ring. The bracket is fixed on the side wall of the cavity by screws, so that the sample can be conveniently put in and taken out.
The invention also discloses a process for carrying out atomic layer deposition reaction by a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes, wherein the atomic layer deposition process comprises the following steps:
step one, heating the cavity (1) to the atomic layer deposition reaction temperature, starting a motor (6), and adjusting the rotating speed;
step two, taking high-purity nitrogen as carrier gas, and pulse-feeding precursor titanium tetrachloride into the cavity (1) through the air inlet pipe (10) and staying for a period of time; precursor gas is uniformly dispersed in the cavity (1) under the rotation and stirring of the hollow fiber membrane (9), fully contacts with the hollow fiber membrane (9), performs monolayer chemical adsorption reaction on the surface of the membrane, then is introduced with nitrogen for 200 seconds to purge excessive reactants and byproducts, and is discharged from the gas outlet pipe (11);
step three, continuing to take high-purity nitrogen as carrier gas, and introducing a precursor oxygen source H 2 O, H 2 O enters the cavity (1) through the air inlet pipe (10) in a pulse mode and stays for a period of time; precursor gas is uniformly dispersed in the cavity (1) under the rotation and stirring of the hollow fiber membrane (9), fully contacts with the hollow fiber membrane (9), performs monolayer chemical reaction with titanium tetrachloride adsorbed on the surface of the membrane, then is introduced with nitrogen for 200 seconds to purge excessive reactants and byproducts, and is discharged from the gas outlet pipe (11); the second step and the third step are completed and then are a cyclic atomic layer deposition reaction;
and step four, after repeating 50-200 times of circulating atomic layer deposition reaction, taking down the upper cover (5), and screws connecting the bracket (8) and the cavity (1), and taking out the porous turntable (2) suspending the hollow fiber membrane (9).
Wherein:
the pulse time of the precursor pulse entering the cavity (1) is 0.1-0.5s, and the residence time is 50-100s. The number of membrane filaments suspending the hollow fiber membrane (9) is 500-1000, and the modified external surface area is 1-2m 2 . The rotating speed adjusting range of the motor (6) is 10-60r/min. The temperature of the cavity (1) for carrying out the atomic layer deposition reaction is 80-150 ℃.
According to the invention, the hollow fiber membrane is fixed on the turntable, and the sample membrane is driven to rotate by adjusting the rotating speed of the motor, so that reactants pulsed into the cavity are uniformly diffused in the cavity, and the reactants are uniformly deposited on the surface of the membrane. The throughput can be increased by increasing the cavity size. The rotational speed can be adjusted to accommodate different deposition conditions.
The beneficial effects are that:
1. by enlarging the reaction cavity, the filling area of the membrane is increased, the loading capacity of the hollow fiber membrane is increased, and the yield and efficiency are improved;
2. the deposition reaction adopts the principle of magnetic force induction, and the reactant is uniformly diffused by rotating the sample, so that the reactant is uniformly adsorbed on the surface of the film, the problem of uneven adsorption due to standing of the substrate is avoided, and the deposition uniformity is ensured.
3. The rotation adopts the principle of magnetic force induction, so that an extra stirring system is prevented from being added in the cavity. Realize batch production and improve production efficiency.
Drawings
Fig. 1 is a front view of the apparatus of the present invention. 1: cavity, 2: porous carousel, 3: magnet, 4: sealing ring, 5: upper cover, 6: a motor, 7: rotating shaft, 8: and (3) a bracket, 9: hollow fiber membrane, 10: intake pipe, 11: and an air outlet pipe.
Fig. 2 is a left side view of the apparatus of the present invention.
Fig. 3 is a top view of the apparatus of the present invention.
FIG. 4 is a schematic diagram of a multi-well turntable of the apparatus of the present invention.
FIG. 5 is an SEM image of hollow fiber membranes batchwise modified by a rotary atomic layer deposition reactor in example 1, and FIG. a is a raw membrane; the b-d plots were deposited 50 times, 100 times, 200 times, respectively.
FIG. 6 is a graph showing the deposition of TiO on a silicon wafer obtained by varying the number of deposition reactions in example 1 2 The deposition reaction times are respectively 50 times, 100 times, 150 times and 200 times.
Detailed Description
The invention will be further explained with reference to examples. The following examples are only illustrative of the present invention and are not intended to limit the scope of the invention.
A rotary atomic layer deposition reactor for batch modification of hollow fiber membranes comprises a cavity (1) and an upper cover (5), wherein the top of the cavity (1) is connected with the upper cover (5) in a sealing way through a sealing ring (4), and an air inlet pipe (10) and an air outlet pipe (11) are arranged at the bottom of the cavity (1); a motor (6) with a magnet (3) is fixed at the top of the upper cover (5), and the motor (6) drives the magnet (3) to rotate through a rotating shaft (7); the same magnet (3) is arranged in the cavity (1), and the magnet (3) in the cavity (1) rotates along with the rotation of the motor (6) under the interaction force of the magnet; the bracket (8) is fixed on the side wall of the cavity (1), and the magnet (3) is fixed on the bracket (8) through the rotating shaft (7); the tail end of the rotating shaft (7) is connected with the porous rotary table (2), and the hollow fiber membrane (9) is hung on the porous rotary table (2). The arrangement of holes in the porous rotary table (2) is concentric circle arrangement, and the hollow fiber membrane (9) is hung on the porous rotary table (2) through a raw material belt. The sealing ring (4) is a fluororubber O-shaped sealing ring. The bracket (8) is fixed on the side wall of the cavity (1) by screws.
Firstly, a porous rotary table (2) and a magnet (3) are fixed on a bracket (8) through a rotating shaft (7), and a hollow fiber membrane (9) is hung on the porous rotary table (2). The bracket (8) is fixed in the cavity (1) by a screw, the sealing ring (4) is arranged at the top of the cavity, and the upper cover (5) provided with the motor (6) is arranged on the cavity (1) so as to achieve the sealing effect. The motor (6) is turned on to enable the magnet (3) to rotate, the porous rotary table (2) connected with the magnet (3) is driven to rotate, the hollow fiber membrane (9) starts to rotate, and vacuumizing and deposition experiments are carried out after the rotating speed is regulated.
Example 1
Suspending hollow fiber membrane (9) on porous rotary disc (2), placing into cavity (1), arranging 500 membrane filaments, and modifying with external surface area of 1m 2 . The rotation speed of the motor is regulated to be 20r/min, the temperature of the cavity body 1 is increased to 100 ℃, and the temperature is kept for 60min, so that the temperature and the pressure in the cavity body (1) are kept stable. Precursor A (titanium tetrachloride) and oxygen source B (H) 2 O) are respectively put into precursor steel cylinders and stored at normal temperature. The flow rate of nitrogen is 30sccm, and the two precursors respectively carry out atomic layer deposition reaction by taking high-purity nitrogen as carrier gas. Firstly introducing titanium tetrachloride to perform atomic layer deposition reaction on the surface of a hollow fiber membrane (9), and then introducing an oxygen source H 2 O performs atomic layer deposition reaction on the surface of the hollow fiber membrane (9). In order to measure the deposition effect of different positions of the cavity (1), silicon wafers are hung at three different positions of the upper, middle and bottom of the cavity (1) and atomic layer deposition reaction is performed simultaneously.
Firstly, titanium tetrachloride is pulsed into a cavity (1) from an air inlet (10), the pulse time of a precursor is 0.25s, the residence time is set to be 50s, and the precursor gas is uniformly dispersed in the cavity (1) under the rotation and stirring of a hollow fiber membrane (9) and is fully contacted with the hollow fiber membrane (9), so that the monolayer chemisorption reaction occurs on the surface of the membrane. After the deposition reaction, the excess reactants and byproducts were purged with nitrogen, which was set to 200 seconds, and discharged from the gas outlet pipe (11) to the system. Then let in H 2 O performs atomic layer deposition reaction under the same conditions, H 2 O is pulsed into the cavity (1) from the air inlet (10), the precursor pulse time is 0.25s, the residence time is set to be 50s, then nitrogen is introduced to purge, and the purge time is set to be 200s. Titanium tetrachloride and H 2 O is respectively subjected to atomic layer deposition and then is subjected to atomic layer deposition reaction for completing one cycle. The atomic layer deposition reactions were repeated 50, 100, 150, 200 cycles. After the experiment is finished, the upper cover is taken down5) And then the screw connecting the bracket (8) and the cavity (1) is taken down, and the porous rotary table (2) hung with the hollow fiber membrane (9) is taken out.
Fig. 5 is an SEM image of a hollow fiber membrane (9) batch-modified by a rotating atomic layer deposition reactor in this example, and it can be seen that some small particles appear on the surface gradually as the number of deposition times increases. The deposition times continue to increase, the film surface is gradually covered by nano particles, and TiO 2 Successfully deposited on the surface of the hollow fiber membrane (9). And the thickness of the deposition layer can be accurately regulated and controlled by controlling the cycle times of atomic layer deposition.
FIG. 6 shows TiO after various deposition reactions in this example 2 Deposition thickness on the surface of the silicon wafer. Calculated as deposited TiO 2 The growth rate of the silicon wafer surface is about 1.5A/cycle, the deposition thickness difference at different positions is smaller at the same deposition times, and the deposition is more uniform in an error range.
Example 2
The atomic layer deposition process was the same as in example 1, except that the process conditions were: the number of membrane filaments of the suspended hollow fiber membrane (9) is 800, and the modified external surface area is 1.5m 2 . The rotation speed of the motor is regulated to 10r/min, and the temperature of the cavity (1) is 150 ℃. The precursor pulse time was 0.5s and the residence time was set to 80s.
Example 3
The atomic layer deposition process was the same as in example (1), except that the process conditions were: the number of membrane filaments of the suspended hollow fiber membrane (9) is 1000, and the modified external surface area is 2m 2 . The rotation speed of the motor is regulated to be 60r/min, and the temperature of the cavity (1) is 80 ℃. The precursor pulse time was 0.1s and the residence time was set to 100s.
Claims (9)
1. The rotary atomic layer deposition reactor for batch modification of hollow fiber membranes is characterized by comprising a cavity (1) and an upper cover (5), wherein the top of the cavity (1) is connected with the upper cover (5) in a sealing way through a sealing ring (4), and an air inlet pipe (10) and an air outlet pipe (11) are arranged at the bottom of the cavity (1); a motor (6) with a magnet (3) is fixed at the top of the upper cover (5), and the motor (6) drives the magnet (3) to rotate through a rotating shaft (7); the same magnet (3) is arranged in the cavity (1), and the magnet (3) in the cavity (1) rotates along with the rotation of the motor (6) under the interaction force of the magnet; the bracket (8) is fixed on the side wall of the cavity (1), and the magnet (3) is fixed on the bracket (8) through the rotating shaft (7); the tail end of the rotating shaft (7) is connected with the porous rotary table (2), and the hollow fiber membrane (9) is hung on the porous rotary table (2).
2. A rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 1, wherein the holes in the porous turntable (2) are arranged in concentric circles, and the hollow fiber membranes (9) are suspended on the porous turntable (2) by a raw material belt and placed in the reaction cavity (1).
3. A rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 1, wherein the sealing ring (4) is a fluororubber O-ring.
4. A rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 1, characterized in that the support (8) is screwed onto the side wall of the chamber (1).
5. A process for carrying out an atomic layer deposition reaction in a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to any one of claims 1 to 4, wherein the atomic layer deposition steps are as follows:
step one, heating the cavity (1) to the atomic layer deposition reaction temperature, starting a motor (6), and adjusting the rotating speed;
step two, taking high-purity nitrogen as carrier gas, and pulse-feeding precursor titanium tetrachloride into the cavity (1) through the air inlet pipe (10) and staying for a period of time; precursor gas is uniformly dispersed in the cavity (1) under the rotation and stirring of the hollow fiber membrane (9), fully contacts with the hollow fiber membrane (9), undergoes a monomolecular layer chemical adsorption reaction on the surface of the membrane, is introduced with nitrogen for 200 seconds to purge excessive reactants and byproducts, and is discharged from the gas outlet pipe (11);
step three, continuing to supply the precursor oxygen source H 2 O, H is carried out by taking high-purity nitrogen as carrier gas 2 O enters the cavity (1) through the air inlet pipe (10) in a pulse mode and stays for a period of time; the surface of the film is subjected to monolayer chemical reaction, then nitrogen is introduced for 200 seconds to purge excessive reactants and byproducts, and the excessive reactants and byproducts are discharged from an air outlet pipe (11) to the system; step two and step three are a cyclic atomic layer deposition reaction after finishing;
and step four, after repeating 50-200 times of circulating atomic layer deposition reaction, taking down the upper cover (5), and screws connecting the bracket (8) and the cavity (1), and taking out the porous turntable (2) suspending the hollow fiber membrane (9).
6. The process for carrying out an atomic layer deposition reaction in a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 5, wherein the pulse time of the precursor pulse into the cavity (1) is 0.1-0.5s, and the residence time is 50-100s.
7. The process for carrying out atomic layer deposition reaction by using a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 5, wherein the number of membrane filaments suspending the hollow fiber membranes (9) is 500-1000 and the modified external surface area is 1-2m 2 。
8. The process for carrying out an atomic layer deposition reaction in a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 5, wherein the rotation speed of the motor (6) is adjusted within the range of 10-60r/min.
9. The process for carrying out an atomic layer deposition reaction in a rotary atomic layer deposition reactor for batch modification of hollow fiber membranes according to claim 5, wherein the temperature of the chamber (1) for carrying out the atomic layer deposition reaction is 80-150 ℃.
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