JPH0615221A - Method for manufacturing monomolecular built-up film - Google Patents

Abstract

PURPOSE:To provide a method for manufacturing a monomolecular built-up film which prevents defects in the structure and orientation of this film on a water level due to a significant turbulence in the water level of a subphase from occurring. CONSTITUTION:This method for manufacturing a monomolecular built-up film is to compress a monomolecular film 3 on a subphase 1 at a constant surface pressure, and scoop and transfer the monomolecular film 3 from the subphase 1 to the surface of a solid substrate 5 with the concurrent vertical movement of the solid substrate 5, a required number of times, which is soaked after passage through the film surface of the monomolecular film 3. The solid substrate 5 which is soaked after passing through the film surface of the monomolecular film 3 is continuously moved vertically a required number of times in such a state that the solid substrate 5 is maintained in contact with the subphase 1.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a monomolecular cumulative film, and more particularly to a method for operating a solid substrate for transferring a monomolecular film on a subphase.

[0002]

BACKGROUND OF THE INVENTION 1935, Langmuir, USA.
Blodgett is a monolayer film in which an insoluble monolayer on the surface of water is transferred to the surface of a solid substrate, and the monolayers on the surface of water are stacked on the transferred monolayer to form a monolayer cumulative film. A method for producing a molecular cumulative film was founded.

The monomolecular cumulative film produced by this production method is a Langmuir-Blodgett film or L
An organic ultrathin film, which is abbreviated as B film and whose thickness and orientation can be controlled in the dimension of molecules, has recently attracted attention from the fields of new materials and advanced technologies.

As a method of forming the above-mentioned monomolecular cumulative film, a general LB method (hereinafter referred to as a vertical dipping method) and a horizontal deposition method are widely known. In the vertical dipping method, as shown in FIG. 3, the insoluble monomolecular film 3 on the water surface 8 is compressed to a constant surface pressure, and then the solid substrate 5 soaked through the monomolecular film 3 is continuous. In this method, the monomolecular film 3 on the water surface 8 is transferred to the surface of the solid substrate 5 while vertically moving up and down a required number of times to laminate (accumulate) a monomolecular cumulative film. On the other hand, the horizontal attachment method is a method in which a horizontally supported substrate is brought into contact with a monomolecular film, and the monomolecular film is pulled up and transferred (not shown).

By the way, in the above vertical dipping method, the solid substrate 5 is used.
When there is a large thickness or when the solid substrate 5 has a rectangular parallelepiped shape or a cylindrical shape, there is a serious problem, and this problem will be described below with reference to FIGS. 4 (a), (b) and (c).

In the conventional vertical dipping method, the solid substrate 5 to which the monomolecular film 3 on the water surface 8 has been transferred is completely pulled up from the water surface 8 by the substrate support rod 62. When the shape of 5 is a rectangular parallelepiped shape or a cylindrical shape, even if the lower end surface 5a of the solid substrate 5 is slightly pulled up from the water surface 8 as shown in FIG. It did not separate from the lower end surface 5a of the substrate 5.

When the solid substrate 5 is further pulled up in this state, water is further sucked between the water surface 8 and the lower end surface 5a of the solid substrate 5, as shown in FIG. 4 (b).
When the solid substrate 5 is continuously pulled up in this suction state, as shown in FIG. 4C, the sucked water rapidly separates from the surface of the lower end 5a of the solid substrate 5 due to its own weight. However, there is a problem that the water surface 8 is greatly undulated and causes defects in the structure and orientation of the monomolecular film 3 on the water surface 8.

This turbulence on the water surface 8 was not a problem in the vertical dipping method in which a slide glass having a thickness of about 1 mm was used as a substrate for a monomolecular cumulative film, but it was a prism or a substrate for liquid crystal cells. Since many solid substrates 5 requiring optical accuracy have a thickness of several millimeters to 1 cm or more, when the monomolecular film 3 is laminated on the solid substrate 5 by the vertical dipping method, Since water is easily sucked by the lower end surface 5a, the water surface 8 is disturbed, which causes a defect in the structure and orientation of the monomolecular film 3 on the water surface 8. Then, such disorder of the structure and orientation of the monomolecular film 3 is inevitably a great obstacle when the monomolecular cumulative film is used as the liquid crystal alignment film or the electronic material.

[0009]

The vertical dipping method in the conventional method for producing a monomolecular cumulative film is performed as described above, and no matter how slow the rising speed of the solid substrate 5, the solid substrate 5 can be made.
After being pulled up from the water surface 8 to a predetermined height, the water rapidly separates from the lower end surface 5a of the solid substrate 5 due to its own weight.
There is a big problem that a serious defect occurs in the structure and orientation of the upper monomolecular film 3.

In other words, the monolayer of the monolayer 3 is disturbed by the large wave of the water surface 8 (two layers and three layers are formed) and cannot be returned to its original state. However, it was impossible to form a clean and high-quality monomolecular film 3 on the solid substrate 5. Then, such disorder of the structure and orientation of the monomolecular film 3 is inevitably a great obstacle when the monomolecular cumulative film is used as the liquid crystal alignment film or the electronic material.

The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a method for producing a monomolecular cumulative film capable of preventing defects in the structure and orientation of the monomolecular film on the water surface due to large disturbance of the water surface. .

[0012]

In order to achieve the above-mentioned object in the present invention, a solid substrate in which a monomolecular film on a subphase is compressed to a constant surface pressure and dipped through the film surface of the monomolecular film. In a method for producing a monomolecular cumulative film by transferring the monomolecular film on the sub-phase to the surface of the solid substrate while moving up and down a plurality of times,
It is characterized in that the above-mentioned solid substrate, which has been soaked through the film surface of the monomolecular film, is moved up and down while being kept in contact with the subphase.

[0013]

According to the present invention, the immersed solid substrate is stopped at the same level as the water surface of the sub-phase or at a position slightly lower than the water surface of the sub-phase, and again immersed in the sub-phase after a predetermined time has elapsed. Since the monomolecular film on the sub-phase is transferred, the solid substrate is constantly in contact with the sub-phase, and with separation of the sub-phase, the water surface of the sub-phase is greatly disturbed and the mono-molecular film on the water surface is disturbed. The problem of causing defects in the structure and orientation can be solved.

[0014]

EXAMPLES The present invention will be described in detail below with reference to one example shown in FIGS. 1 and 2. In the method for producing a monomolecular cumulative film according to the present invention, the film of the insoluble monomolecular film 3 on the subphase 1 is formed. The solid substrate 5 soaked through the surface is vertically moved up and down a required number of times while being kept in contact with the sub-phase 1 to laminate-produce a monomolecular cumulative film made of the same substance.

As shown in FIG. 1, the subphase 1 (the liquid phase supporting the insoluble monomolecular film 3) is made of water, an aqueous solution or the like, and is stored inside the liquid tank 2. A partition plate 4 for maintaining the monomolecular film 3 formed on the sub-phase 1 at a constant surface pressure is arranged on the upper right side of the inside. In addition, although the sub-phase 1 made of water, an aqueous solution or the like is shown in this embodiment, the sub-phase 1 made of a non-aqueous solution of methanol, ethanol, acetone, glycerin, mercury or the like may be used.

The solid substrate 5 is suspended by a solid substrate elevating mechanism 6 located on the upper left side of the liquid tank 2 so as to be vertically movable, and the solid substrate elevating mechanism 6 is controlled by a controller 7 programmed in advance. It has a function of immersing the solid substrate 5 in the subphase 1 in the liquid tank 2 by operating based on the above.

As shown in FIG. 1, the solid substrate up-and-down mechanism 6 is provided with a motor 60 which is rotationally driven at a low speed under the control of the controller 7, and the rotation shaft of the motor 60 has a pinion 6.
1, the rack 63 on the upper side of the substrate support rod 62 oriented in the vertical direction is meshed with the pinion 61, and the clip 64 on the lower end of the substrate support rod 62 is engaged.
The solid substrate 5 is suspended in the.

Then, as shown in FIG. 2, the controller 7 immerses the solid substrate 5 in the sub-phase 1 in the liquid tank 2 from the basic position above the liquid tank 2, and then, unlike the conventional example, the sub-phase 1 It is pre-programmed to vertically move the solid substrate 5 immersed through the film surface of the upper monomolecular film 3 up and down a required number of times while being kept in contact with the subphase 1. Therefore,
It is important to detect the relative position of the solid substrate 5 and the subphase 1,
The relative position between the solid substrate 5 and the subphase 1 is numerically input to the controller 7, regulated by a mechanical stopper (not shown), or confirmed by a light source and a photodetector (not shown).

Therefore, in order to manufacture a monomolecular cumulative film, the solid substrate elevating mechanism 6 may be operated. Then, the motor 60 is rotationally driven at a low speed under the control of the controller 7 to rotate the pinion 61, and the substrate support rod 62 in which the rack 63 is meshed with the pinion 61 is lowered to basically suspend the solid substrate 5. The monomolecular film 3 on the subphase 1 is transferred to the surface of the solid substrate 5 by passing the film surface of the monomolecular film 3 from the position and immersing the subphase 1 in the liquid tank 2 at an extremely low speed. Since the solid substrate 5 is immersed in the subphase 1 in the liquid tank 2 at an extremely low speed, the disturbance of the monomolecular film 3 on the subphase 1 can be reliably prevented.

Next, the solid substrate 5 which has been dipped through the film surface is continuously vertically moved up and down a required number of times, and then the solid substrate 5 is immersed.
The monomolecular film 3 on the sub-phase 1 is transferred to the surface of the substrate to laminate (cumulatively) manufacture a monomolecular cumulative film. However, unlike the conventional example, the rising solid substrate 5 is as shown by the dotted line in FIG. Subphase 1
The surface of the sub-phase 1 is stopped at a level equal to or lower than the surface of the sub-phase 1, and after a lapse of a predetermined time, the sub-phase 1 is immersed again to transfer the monomolecular film 3 on the sub-phase 1.

However, the operation of vertically moving up and down in the state of being in contact with the sub-phase 1 of the solid substrate 5 is continuously repeated a required number of times until the stacking of the monomolecular cumulative film is completed. In this way, when the stacking of the monomolecular accumulated film is completed, the solid substrate 5 is transported from the liquid tank 2 to the next step (not shown).

According to the above method, the immersed solid substrate 5
Stops on the same level as the water surface of the sub-phase 1 or slightly below the water surface of the sub-phase 1, and after a predetermined time elapses, is immersed again in the sub-phase 1 to transfer the monomolecular film 3 on the sub-phase 1. Therefore, the solid substrate 5 is constantly in contact with the subphase 1,
It is possible to solve the problem that the water surface of the sub-phase 1 is greatly disturbed due to the separation of the sub-phase 1 and a defect occurs in the structure and orientation of the monomolecular film 3 on the water surface.

More specifically, it is possible to prevent the monomolecular layer of the monomolecular film 3 from being disturbed (two-layered and three-layered portions are formed) due to the large waviness of the subphase 1 and being disturbed. It is possible to eliminate the condition that the monolayer must be deposited on the solid substrate 5, and a clean and high-quality monomolecular film 3 is formed on the solid substrate 5.
Can be easily created.

Therefore, even for the thick solid substrate 5 made of an optical material or the like, or the solid substrate 5 having a rectangular parallelepiped shape or a cylindrical shape,
The monomolecular film 3 having no defect in structure or orientation can be laminated very easily. The disturbance of the monolayer due to the large wave of the water surface of the sub-phase 1 cannot be prevented even if the rising speed of the solid substrate 5 is slowed down. Therefore, the present invention is extremely useful in producing a high-quality monomolecular cumulative film. It is valid.

Next, the experimental results of the method for producing a monomolecular cumulative film according to the present invention will be specifically described in comparison with the conventional prior art. As disclosed in JP-A-3-164655, the polysilane derivative monomolecular cumulative film effectively functions as a liquid crystal alignment film in a ferroelectric liquid crystal device.

However, in the conventional manufacturing method, if a thick substrate (35 mm × 30 mm × 5 mm) is used,
It was confirmed by polarization microscope photographs that the orientation of the polysilane derivative monomolecular cumulative film was disturbed, and in the ferroelectric liquid crystal device using the orientation film, the liquid crystal device was significantly disturbed.

On the other hand, in the ferroelectric liquid crystal device using the polysilane derivative monomolecular cumulative film manufactured by the method for manufacturing a monomolecular cumulative film according to the present invention as the alignment film, the liquid crystal alignment is significantly improved. Was clearly confirmed by a polarization micrograph.

In the above embodiment, the monomolecular film 3 made of the same substance is laminated, but it is also applicable to a composite cumulative film produced by laminating plural kinds of monomolecular films. Further, in the above embodiment, the solid substrate up-and-down mechanism 6 is operated to move the solid substrate 5 up and down, but the solid substrate up-and-down mechanism 6 having the above structure is not limited.

[0029]

As described above, according to the present invention, the immersed solid substrate stops at the same level as the water surface of the sub-phase or slightly lower than the water surface of the sub-phase, and again after a predetermined time elapses. Since the monolayer on the sub-phase is transferred by being immersed in the phase, the solid substrate is constantly in contact with the sub-phase, and the water surface of the sub-phase is greatly disturbed due to the separation of the sub-phase. There is a remarkable effect that the problem of causing a serious defect in the structure and orientation of the upper monolayer can be surely solved.

In detail, it is possible to surely prevent the monomolecular layer from being disturbed and unable to return to its original state due to a large wave of the sub-phase, and the disordered monomolecular layer must be deposited on the solid substrate. Can be easily eliminated, and it is possible to form a clean and high quality monomolecular film on a solid substrate very easily.

Therefore, a monomolecular film having no defect in structure or orientation can be very easily laminated on a thick solid substrate made of an optical material or the like or a solid substrate having a rectangular parallelepiped shape or a cylindrical shape. It has a remarkable effect. Since the disturbance of the monolayer due to the large waviness of the water surface of the subphase cannot be prevented by slowing the rising speed of the solid substrate, the present invention is extremely effective in producing a high quality monomolecular cumulative film. Be effective.

[Brief description of drawings]

FIG. 1 is an overall explanatory view showing an example of a method for producing a monomolecular cumulative film according to the present invention.

FIG. 2 is an explanatory view of a principal part showing an embodiment of a method for producing a monomolecular cumulative film according to the present invention.

FIG. 3 is a principal part explanatory view showing a vertical dipping method in a conventional method for producing a monomolecular cumulative film.

FIG. 4 is an essential part explanatory view showing a defect of the vertical dipping method in the conventional method for producing a monomolecular cumulative film.

[Explanation of symbols]

1 ... Subphase, 2 ... Liquid tank, 3 ... Monomolecular film, 4 ... Partition plate, 5
... solid substrate, 6 ... solid substrate up-and-down mechanism, 7 ... controller.

 ─────────────────────────────────────────────────── ─── Continuation of front page (72) Inventor Toshiaki Ito 1126-1 Nomachi, Hamamatsu-shi, Shizuoka 1 Hamamatsu Photonics Co., Ltd.

Claims (1)

[Claims] 1. A monolayer on the subphase is compressed on a surface of the subphase by compressing the monolayer on the subphase to a constant surface pressure, and raising and lowering a solid substrate which has been immersed and passed through the surface of the monolayer a plurality of times. In the method for producing a monomolecular cumulative film by transferring a molecular film to produce a monomolecular cumulative film, the solid substrate immersed through the film surface of the monomolecular film is moved up and down while being in contact with the subphase. A method for producing a monomolecular cumulative film, comprising: