JPH055682A - Treatment method and device for making hydrophilic for microtome knife - Google Patents

Abstract

PURPOSE:To easily make hydrophilic in a short time by arranging carbon or aluminum on discharge electrodes of a vacuum vessel as a target material, placing a knife for a microtome and applying voltage across the discharge electrodes. CONSTITUTION:A knife 27 is set on a microtome knife base 30, an edge of the knife 27 is positioned in a vacuum vessel 20 and the angle of the edge can be changed by operating a lug 29 of the base 30. The vessel 20 is supported with a support rod 31, a negative electrode 21 and a positive electrode 22 are provided in the inside thereof, and a carbon plate 23 is attached to the negative electrode 21 as a target. Voltage is applied from a power source 34. After a rotary pump 32 is started by the control of a controller 33, the power source 34 is switched on to start glow discharge between the electrodes 21, 22 when a degree of vacuum reaches a specified value. After a controller 33 built-in timer is operated and discharge is performed during a specified time, the power source 34 is switched off. As the result the glow discharge is generated during the specified time alone by the operation of the controller 33 and hydrophile treatment can be performed automatically.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and apparatus for hydrophilizing a microtome knife having improved hydrophilicity.

[0002]

2. Description of the Related Art As shown in FIG. 4, a knife for a microtome used for preparing a sample for an electron microscope has a water reservoir boat 4 filled with water formed on an upper portion of a main body 2 and a cutting edge 3 at an end thereof. The structure is provided. When producing an ultrathin section with such a microtome, as shown in FIG. 5, the sample 7 attached to the tip of the extension rod 6 is mechanically fed by a mechanism (not shown) or advanced by a thermal expansion method. As a result, the knife 3 cuts out the portion that has been sent. The cut section 8 floats on the surface of the water 5 contained in the water reservoir boat 4 of the knife 1, and this section is placed on a grid to be used as a sample for an electron microscope.

[0003]

By the way, the microtome knife used for producing an ultrathin section is generally made of glass or diamond. Although diamond knives are expensive, they tend to be used more often because they have excellent characteristics that glass does not have, such as durability and the ability to cut hard materials. Such a diamond knife is not disposable, and one knife has been used for many years, and tends to become hydrophobic as it is used. When the knife becomes hydrophobic, even if the boat is filled with water at an appropriate level, the blade repels the water, and the water does not reach the blade as shown in FIG. 6A. If the sample is cut in this state, the sliced pieces will become crumpled and stick to each other, making them unusable as sliced pieces. Also, FIG. 6 (b)
When the water level is set so that the tip of the water raised by the surface tension reaches the cutting edge as shown in (4), water adheres to the sample surface and cutting cannot be performed. Therefore, as shown in Fig. 6 (c), it is necessary for the water surface to the knife so that the water surface does not rise at the cutting edge so that the tip of the water reaches the cutting edge. For that purpose, the blade must be hydrophilic. I have to. In this way, in order to make the blade hydrophilic,
Conventionally, a hydrophilizing agent is added to water in a boat for hydrophilization treatment.

The knife is submerged in water overnight before use.

Wash with a neutral detergent.

And so on. However, in the method of, it is difficult to add the hydrophilic agent, and even if an appropriate amount of water is put in the boat, the water is easily drawn into the back of the knife and the sample surface, and the effect disappears when the water is replaced several times,
The method (2) takes time and cannot be used immediately when desired, and the effect is lost when dried, and the method (2) has a problem that the effect is not remarkable and the reproducibility is poor.

The present invention has been made to solve the above-mentioned problems. It can be easily hydrophilized in a short time without using a hydrophilizing agent, and the hydrophilic effect can be maintained for a long time. An object of the present invention is to provide a knife hydrophilization treatment method and apparatus in which water is not drawn into a sample surface.

[0008]

According to the present invention, carbon or aluminum is placed as a target material on a discharge electrode in a vacuum vessel, and a microtome knife is placed on the discharge electrode to apply a voltage between the discharge electrodes. A method for hydrophilizing a microtome knife that causes a discharge to hydrophilize the microtome knife, and a predetermined voltage is applied from a power source, and a discharge electrode having a target placed on at least one of them is disposed, and at least a microtome knife A vacuum container configured such that the blade edge thereof is located inside, an exhaust unit for exhausting the vacuum container, a measuring unit for measuring the degree of vacuum, a power source, an exhaust unit, a measuring unit, and a timer can be set. A control device is provided, and a glow discharge is generated between the discharge electrodes for a predetermined time by the control of the control device. DOO characterized microtome knife hydrophilic treatment device according to claim.

[0009]

According to the present invention, the target voltage is 250 to 300 in a vacuum container containing a carbon or aluminum target.
V, ion current 3 to 5 mA, discharge time 5 to 20 seconds, and vacuum degree of about 10 PA are caused to cause glow discharge to be hydrophilic. By such a treatment, the hydrophilic treatment can be easily performed in a short time and the hydrophilic effect can be maintained for a long time.

[0010]

EXAMPLE FIG. 1 is a diagram for explaining the hydrophilic treatment method of the present invention.

A diamond knife 1 and a horizontal electrode 11 as a carbon target are placed in a vacuum container 10, and a rotary pump (R) (not shown) is supplied from an exhaust pipe 12.
It is evacuated by P), the vacuum in the vacuum container is set to about 10 Pascal (PA), the condition of 3 to 5 mA and the voltage of 250 to 300 V is maintained from the power source 13, and the glow discharge is caused for 5 to 20 seconds. By this glow discharge, the cutting edge of the knife 1 can be made hydrophilic in an extremely short time. When the hydrophilic effect is lost, it can be regenerated many times by similarly causing a glow discharge.

Instead of the diamond knife, a material such as sapphire, ceramic or glass can be used.
Aluminum can also be used as the material of the target.

FIG. 2 shows an example in which a hydrophilic treatment device by glow discharge is attached to an ultramicrotome. In the figure, 20 is a vacuum container, 21 and 22 are electrodes, 23 is a carbon plate, 24 is a Pirani measuring tube, 25 is a leak valve, 26 is an exhaust pipe, 27 is a knife, 28 is a vacuum packing (O-ring), and 29 is Knob, 30 is a microtome knife stand, 3
1 is a support rod, 32 is a rotary pump (RP), 33 is a control device, 34 is a power supply, and 35 is a measuring device.

In the figure, the knife 27 is placed on a microtome knife table 30, the knife edge is located in the vacuum vessel 20, and the angle of the blade can be changed by operating a knob 29 of the microtome knife table 30. Is becoming The vacuum vessel 20 is supported by a support rod 31, a negative electrode 21 and a positive electrode 22 are provided inside, and a carbon plate 23 as a target is mounted on the negative electrode.
00V is applied. Also, the exhaust pipe 26
Is exhausted by RP32 through
The degree of vacuum is measured by a measuring device 35 through the Pirani measuring tube 24, and the RP 32, the power source 34, and the measuring device 35 are controlled by a control device 33 such as a personal computer.

Under control of the control device 33, when the degree of vacuum reaches approximately 10 PA after the start of the RP 32, the 300 V power supply 34 is turned on and the discharge between the electrodes 21 and 22 starts glow discharge. At the same time, a timer built in the control device is activated. The power supply 34 is turned off when it operates and is discharged for 10 seconds, for example. The discharge time is set by the timer of the control device, and the optimum time can be set as appropriate.

As described above, since the glow discharge is generated for a predetermined time by the operation of the control device 33 and the hydrophilic treatment can be automatically performed, the production of the ultrathin section is extremely easy.
And it can be done efficiently.

Further, as shown in FIG. 3, a single hydrophilization treatment device in which the knife is not attached to the microtome knife base may be used. In this case, the knife 43 is directly attached to the vacuum container 40.
It is placed inside and placed on the positive electrode, and high voltage is applied between the negative electrode and the carbon plate to cause glow discharge.

[0018]

As described above, according to the present invention, the hydrophilic effect can be easily obtained in a short time without using a hydrophilizing agent and the like, and the hydrophilic effect can be maintained for a long time. Water will not be drawn into the sample surface. In addition, it can be easily hydrophilized by a fully automatic operation, and the ultrathin section can be efficiently produced.

[Brief description of drawings]

FIG. 1 is a diagram illustrating a hydrophilic treatment of the present invention.

FIG. 2 is a diagram illustrating an embodiment of a hydrophilic treatment device of the present invention.

FIG. 3 is a diagram illustrating another embodiment of the hydrophilic treatment device of the present invention.

FIG. 4 is a diagram illustrating a microtome knife.

FIG. 5 is an explanatory view of cutting out a sample section with a microtome knife.

FIG. 6 is a diagram for explaining hydrophilicity of a cutting edge.

Claims (1)

Claim: What is claimed is: 1. Carbon or aluminum is placed as a target material on a discharge electrode in a vacuum container, and a microtome knife is placed, and a voltage is applied between the discharge electrodes to perform glow discharge. A method for hydrophilizing a knife for a microtome, which is produced by hydrophilizing the knife for a microtome. 2. A vacuum container configured such that a predetermined voltage is applied from a power source, a discharge electrode on which a target is placed is disposed on at least one side, and at least a cutting edge of a microtome knife is located inside. Evacuation means for evacuating the vacuum container, measurement means for measuring the degree of vacuum, and a power source, evacuation means, control means for controlling the measurement means, and a control device capable of setting a timer. A knife hydrophilization treatment device for a microtome, which is characterized in that a glow discharge is generated between them.