KR101076218B1 - Formation apparatus and method thereof of alloy composite membrane - Google Patents

Abstract

According to the present invention, an apparatus for forming an alloy separator by sputter deposition includes: a chamber in which at least one support is loaded, and the deposition is performed on the support; A stage positioned below the chamber and having a supporter to which the support is fixed; A palladium target positioned on the stage and supplying palladium deposited on the support; A metal target positioned on the stage and supplying metal deposited on the support; And a pivot unit connected to the stage to convert the stage to a position corresponding to the palladium target and the metal target, respectively.

Membrane, Palladium, Metal, Support

Description

Alloy Separator Forming Apparatus and Forming Method thereof {FORMATION APPARATUS AND METHOD THEREOF OF ALLOY COMPOSITE MEMBRANE}

The present invention relates to an alloy separator forming apparatus and a method for forming the same, and more particularly, to an alloy separator forming apparatus and a method for forming the same, which can improve productivity when forming a palladium alloy separator by sputtering.

In general, since the separator used in the production of ultra high purity hydrogen has low permeability, it is currently being developed to improve the selective permeability of the membrane by coating a non-porous palladium membrane on the porous support. However, non-porous palladium membranes have good selectivity for hydrogen (H ₂ ) but low permeability. Therefore, although a thin palladium membrane is coated on the surface of the porous support to increase the permeability of hydrogen selectively, in the case of a separator using palladium only, there is a problem that deformation occurs due to phase transformation of the lattice due to absorption of hydrogen gas. In order to prevent this, palladium alloy separators are used a lot now.

Such palladium alloy separators are formed by electroless plating, chemical vapor deposition, electrodepostion, sputtering, spray pyrolysis and wet impregnation. depostion), and appropriate methods are used depending on the properties, materials, and support properties required for thin films.

In particular, the sputtering method is a method in which a metal of high energy ions striking a metal target is deposited on a support and formed into a thin film. The sputtering method produces a metal film quickly and has an advantage of easy control of thickness.

However, when the palladium alloy separator is formed, the temperature must be lowered prior to the extraction of the separator according to the temperature rise in the chamber. Therefore, productivity improvement is emerging as a key factor in considering the temperature drop time.

The present invention has been made in order to solve the above problems, the object of the present invention is to form a palladium alloy separation membrane to support a plurality of supports to the support support to be able to be produced in large quantities by sequentially depositing palladium and metal sequentially An alloy separator forming apparatus and a method of forming the same are provided.

According to the present invention, an apparatus for forming an alloy separator by sputter deposition includes: a chamber in which at least one support is loaded, and the deposition is performed on the support; A stage positioned below the chamber and having a supporter to which the support is fixed; A palladium target positioned on the stage and supplying palladium deposited on the support; A metal target positioned on the stage and supplying metal deposited on the support; And a pivot unit connected to the stage to convert the stage to a position corresponding to the palladium target and the metal target, respectively.

The supporter may have a plurality of grooves in which the support is installed, and the grooves may be positioned at an angle with respect to the rotation center of the stage.

The alloy separator may further include a target cover to selectively block any one of the palladium target and the metal target.

A plurality of supports are fixed on the support support to form a conformal angle with respect to the rotation center of the stage, the rotating portion may rotate the support support by the angle formed by the support.

The rotating part includes a driving shaft connected to the stage and rotating together with the stage, and an interference member installed on the driving shaft and rotating together with the driving shaft, wherein the alloy separator forming apparatus is installed around the driving shaft to provide the interference member. It may further include a sensor for detecting the position of.

Meanwhile, the metal may be copper.

According to one embodiment of the present invention, a method of forming an alloy separation film by sputter deposition comprises the steps of installing a support on a support support installed in the chamber; Rotating the support support to move the support to a position corresponding to the palladium target and depositing a palladium coating layer on the support; And rotating the support holder to move the support to a position corresponding to the metal target and depositing metal on the palladium coating layer.

According to another embodiment of the present invention, a method of forming an alloy separation film by sputter deposition includes the steps of installing a plurality of supports on a support support installed in the chamber; Rotating the support support to sequentially move the support to a position corresponding to the palladium target and sequentially depositing a palladium coating layer on the support; And rotating the support holder to sequentially move the support to a position corresponding to the metal target and sequentially depositing metal on the palladium coating layer.

Blocking the metal target in the step of depositing the palladium coating layer, and blocking the palladium target in the step of depositing the metal.

Such an alloy separator forming apparatus and a method of forming the same according to the present invention, by forming a palladium alloy separator is fixed to a plurality of supports on the support base to sequentially deposit the palladium and the metal has the effect that can be produced in large quantities.

Hereinafter, with reference to the accompanying drawings, the alloy separator forming apparatus and the method of forming the present invention will be described with reference to an embodiment as follows.

In the alloy separator forming apparatus according to an exemplary embodiment of the present invention, as shown in FIGS. 1 to 3, the palladium film and the metal film are uniformly sequentially deposited on at least one support 140 that is a separator to be formed by a dry vacuum method. And a chamber 100, a target 110, a DC power 118, a stage 120, a rotating unit 130, and a control unit (not shown).

Here, the two-layer film formed on the support 140 is alloyed by a subsequent reflow process to form a palladium-metal alloy separator. This reflow process is preferably carried out in an in-situ manner and may be performed by heat treatment at a set vacuum degree and a set temperature under a hydrogen atmosphere of the chamber 100. The reflow makes the microstructure of the alloy denser and at the same time obtains a uniform separator free from defects and micropores.

The chamber 100 is a sputtering chamber, and a pump is connected to one side in order to convert the interior into a vacuum state, and a gas supply unit and the other side are connected to collide an activation gas ion to a target 110 to be described later. At this time, the inner atmosphere of the chamber 100 is made into a plasma atmosphere, and then palladium particles and metal particles generated by colliding activating gas ions with palladium and metal are supported on the stage 120. In order). Meanwhile, copper is applied to the metal.

The target 110 is installed at the upper end of the chamber 100 and sequentially imparts active gas ions to the neighboring palladium target 112 and the metal target 114 to bring the palladium particles and the metal particles to the support 140. Supply sequentially.

In addition, a target cover 116 is provided at the center of the palladium target 112 and the metal target 114 to rotate by a driving motor to block any one target. This is because the target cover 116 blocks the bottom of one target, so that when the activation gas ions deposit either palladium or metal, the other is not deposited.

The DC power 118 is provided above the chamber 100 to apply a negative voltage to the target 120 and injects a process gas such as argon (Ar) through a gas supply into the chamber 100. Plasma is generated by causing the free electrons accelerated by the electric field to chain collision with gas particles.

That is, the DC power 118 supplies an activation gas which is a process gas into the chamber 100 and then applies an electric field to make the interior of the chamber 100 into a plasma atmosphere.

The stage 120 is provided in the lower side of the chamber 100, but the support support 122 is fixed to the support 140 is fixed to the support 140 is formed on the upper portion of the rotating unit 130 to be described later By aligning the support 140 to form a separator by the target 110 to be described later.

The support support 122 is formed of a disc or the like, and the number of supports 140 while the two points distance to the center of the palladium target 112 and the metal target 114 is the same diameter and the diameter of the circle. As many grooves 124 are formed on the upper surface at equal intervals. At this time, the support 140 in the present invention is illustrated as being provided with four grooves 124 are formed every 90 ° position, the number of the support 140 can be increased or decreased.

Meanwhile, the support 140 is a porous nickel (Ni) support and has excellent chemical affinity with palladium and nickel, which are main components of the palladium alloy composite membrane. The support support 122 is also a nickel support support.

The rotating unit 130 is installed on the bottom of the chamber 100 and rotates the stage 120 having the driving shaft 126 fixed to the bottom by the driving force of the driving motor M. In this case, timing pulleys are respectively installed on the shaft of the driving shaft 126 and the driving motor M parallel thereto, and the driving force of the driving motor M is connected to the driving shaft 126 by interconnecting the timing pulley with a timing belt. To pass.

In addition, an extension member 128 is fixedly installed at the bottom of the chamber 100 at a position perpendicular to the support 140 with respect to the drive shaft 126. At this time, the extension member 128 is provided with the same number of the support body 140, respectively, the optical sensor (S) is installed for each lower end and any one optical sensor with rotation at the lower end of the drive shaft 126 ( The interference member 126a is provided to output the sensing signal at S).

That is, when the supporter 140 is installed at four points by 90 ° on the supporter 122, the extension member 128 is also installed at four points by 90 ° while being perpendicular to the supporter 140. When the drive shaft 126 is rotated by the rotation of the 120, the interference member 126a installed at the lower end of the drive shaft 126 is interlocked so that the emitted light of the sensor S installed at the lower end of the extension member 128 at every 90 ° position cannot be received. To interfere.

As a result, the interference member 126a is also rotated when the stage 120 is rotated by the pivoting unit 130 and blocks the reception of the sensor S installed at the lower end of the extension member 128 according to the signal. Since the control unit controls the driving motor M to stop operating, when the driving motor M stops, the support 140 is positioned perpendicular to the center of the palladium target 112 or the metal target 114. It is possible to deposit only on the support 140.

In the method of forming an alloy separator according to the present invention, as shown in FIGS. 1 to 4, a step of installing a plurality of supports (S150), a step of pumping the inside of a chamber (S152), and a step of continuously depositing palladium on a support (S154) , And continuously depositing a metal on the palladium deposited on the support (S156) and taking out the separator (S158). Here, the metal is copper.

Installing the plurality of supports (S150) is to install a plurality of supports 140 to form a separator on the groove 124 of the support support 122 provided in the stage 120 in the chamber 110, respectively Step.

At this time, before or after the step of installing the plurality of supports (S150) includes the step of mounting palladium and copper to the palladium target 112 and the metal target 114, respectively. And blocking the metal target 114 by operating the target cover 116 to deposit a palladium film in one step.

In the pumping of the inside of the chamber (S152), a chamber (110) is operated by operating a pump (not shown) connected to the chamber 110 for a predetermined time in order to convert the inside of the chamber 110 into a vacuum state at atmospheric pressure. It is a step of evacuating the interior.

Continuously depositing palladium on the support (S154) may sequentially deposit palladium on the plurality of supports 140 by sequentially rotating the support 140 to a position corresponding to the palladium target 112 of the target 110. In this step, when a plasma is generated by applying an electric field through the DC power 118, argon ions collide with the palladium surface of the palladium target 112 on which the cathode is formed, and palladium particles are deposited on the surface of the support 140. Thus, a palladium film is formed.

When the palladium film is deposited on the surface of the first support 140, the rotation angle of the support 140 rotated to a position corresponding to the palladium target 112 is sensed to deposit the palladium film on the surface of the second support 140. The step of aligning is performed, which is driven by the control of the controller to drive the drive shaft 126 driven by the timing belt and the stage 120 and the support support 122 While rotating, the second support 140 installed in the groove 124 of the support support 122 is rotated to a position perpendicular to the palladium target 112.

At this time, the interference member 126a disposed at the lower end of the driving shaft 126 blocks the light reception of the sensor S installed at the corresponding extension member 128 throughout the process of depositing the palladium film on the first support 140. When the deposition process of the film is completed, the control unit of the control unit moves to the sensor S corresponding to the second support 140 and stops the reception of the sensor S and at the same time stops the driving of the driving motor M.

As described above, after the support 140 is aligned, the deposition of the palladium film on the surfaces of the third and fourth supports 140 is sequentially completed by the rotation of the support supports 122.

Continuously depositing the metal on the palladium deposited on the support (S156) is to sequentially rotate the support 140 to a position corresponding to the metal target 114 to continuously deposit the metal on the palladium deposited on the support 140 In the depositing step, the metal film is deposited on the surface of the palladium film in two steps. In this case, the target cover 116 is rotated to block the palladium target 112.

Thereafter, while rotating the support support 122 in the same manner as depositing a palladium film, a metal film of copper is sequentially deposited on the surfaces of the first to fourth supports 140 on which the palladium film is deposited.

That is, when a process gas containing argon gas or the like is injected into the chamber 100, and a plasma is generated by applying an electric field, argon ions collide with the copper surface of the metal target 114 on which the cathode is formed. Particles are deposited on the surface of the support 140 to form a copper film.

Extracting the separator (S158) is a step of taking out the separator after the internal temperature of the chamber 100 is lowered to room temperature for a set time.

In the detailed description of the present invention described above with reference to the preferred embodiment of the present invention, the scope of protection of the present invention is not limited to the above embodiment, and those skilled in the art of the present invention It will be understood that various modifications and changes can be made in the present invention without departing from the spirit and scope of the invention.

1 is a side cross-sectional view showing a state in which a palladium film is formed on a support in the alloy separator forming apparatus according to the present invention.

Figure 2 is a side cross-sectional view showing a state of forming a metal film on the support in the alloy separation film forming apparatus.

3 is a perspective view illustrating a driving unit of the alloy separator forming apparatus.

4 is a flowchart illustrating a method of forming an alloy separator according to the present invention.

<Description of Symbols for Main Parts of Drawings>

100: chamber 110: target

112: palladium target 114: metal target

116: target cover 120: stage

122: support support 124: groove

126: drive shaft 126a: interference member

130: drive unit S: sensor

Claims (9)

In the apparatus for forming an alloy separation film by sputter deposition, A chamber in which a plurality of supports are loaded and the deposition is performed on the supports; A stage positioned below the chamber and having a supporter to which the support is fixed; A palladium target positioned on the stage and supplying palladium deposited on the support; A metal target positioned on the stage and supplying metal deposited on the support; And And a rotating part for rotating the stage so that the plurality of supports are sequentially positioned corresponding to the palladium target and the metal target, respectively. The method of claim 1, The support member has a plurality of grooves in which the support is installed, the grooves are alloy separation film forming apparatus, characterized in that positioned so as to be equal to the center of rotation of the stage. The method of claim 1, The alloy separator forming apparatus further comprises a target cover for selectively blocking any one of the palladium target and the metal target. The method of claim 1, A plurality of supports are fixed on the support support at an equilibrium with respect to the rotation center of the stage, And the pivoting part rotates the supporter by an angle formed by the supports. The method of claim 1, The rotating part includes a driving shaft connected to the stage and rotating together with the stage, and an interference member installed on the driving shaft and rotating together with the driving shaft. The alloy separator forming apparatus further comprises a sensor installed around the drive shaft for sensing the position of the interference member. The method of claim 1, The metal is an alloy separator, characterized in that the copper. delete In the method of forming an alloy separation film by sputter deposition, Installing a plurality of supports on a support support installed in the chamber; Step-rotating the support supports to sequentially move the supports to positions corresponding to the palladium targets, respectively, and sequentially depositing a palladium coating layer on each support; And Step-rotating the support support to sequentially move the support to a position corresponding to each of the metal targets, and sequentially depositing a metal on the palladium coating layer. The method of claim 8, Blocking the metal target in depositing the palladium coating layer, And depositing the metal to block the palladium target.

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