JP2004358208A - Production method, production equipment, and continuous production equipment for ceramic-coated needle - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To enable a ceramic-coated needle with excellent coating film adhesion and little coating unevenness to be provided at a low price. <P>SOLUTION: When a coating of a ceramic film is applied at least on the tip part of a needle made of a metal by a dry plating method, the metal needle is set in parallel with the direction of advancing deposited particles while the tip part thereof is made to face the advancing deposited particles. Holding this position, the metal needle is made to have a back and forth movement and crisscross movement against the traveling direction of the deposited particles, a rotational movement making the traveling direction as its rotational axis, or an revolutional and rotational movement with a horizontal or vertical axis against the traveling direction while it is coated with the ceramic. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method, a manufacturing apparatus, and a continuous manufacturing apparatus for ceramic coated needles such as medical coated needles such as injection needles and puncture needles and ceramic coated needles for gene control.

  In recent years, medical technology has made remarkable progress. For example, in the examination of the liver and pancreas, etc., in order to obtain data that cannot be obtained by a patient's blood test, an ultrasonic examination using an echo or a CT (computed tomography) examination MRI (Magnetic Resonance Imaging), which uses a strong magnetic field and radio waves to project cross-sectional images of various organs, and angiography, which injects a contrast agent through a thin tube (catheter) and images the state of blood vessels, etc. Widely used.

According to these blood tests and various types of image diagnosis, the presence of a lesion such as a cancer can be diagnosed, but for a definitive diagnosis, histopathological examination of a lesion by a liver biopsy or the like is required.
Usually, in such an examination, a method is employed in which a special puncture needle is directly pierced into a lesion to collect a tissue piece.

However, when a current metal puncture needle is used, the base material of the needle is a conductive metal having excellent electrical characteristics (resistivity ρ: 10 ⁻⁶ to 10 ⁻⁸ Ω · m). It has been pointed out that the cells around the puncture needle pierced into a tissue piece or a lesion taken from a bacterium have an adverse effect.

In this regard, it is considered that the use of the ceramic puncture needle does not adversely affect the cells around the puncture needle pierced into the collected tissue piece or lesion.
However, ceramic puncture needles are very fragile and easily broken, so they are not used at present.

As a solution to the above-mentioned problem, the inventors have previously stated that `` a metal needle has an insulating ceramic coating having a resistivity ρ of 10 ⁵ Ωm or more on part or all of its surface. "Characterized ceramic coated needle for medical use" has been developed (for example, see Patent Document 1).
With the development of the above technology, it has become possible to collect a tissue piece without causing breakage or the like during use and without adversely affecting cells around a puncture needle punctured in a lesion. .

As described above, a ceramic-coated needle having a ceramic coating having excellent insulating properties has a very small adverse effect on living tissues and cells.
Thus, the present inventors have conducted studies over a wide range of technical fields in order to utilize the above-mentioned features of the ceramic-coated needle in fields other than medical use, and as a result, have found a particularly excellent effect in the field of gene regulation. And newly developed a ceramic-coated needle for gene control (see, for example, Patent Document 2).

However, even when the above-mentioned ceramic-coated puncture needle is used, there is a case where the collected tissue piece has an adverse effect.
That is, since the outer surface of the puncture needle was covered with an insulating ceramic, the cells around the puncture needle punctured the lesion were not damaged at all, but the inside of the puncture needle was not damaged. Since it is not always coated with such insulating ceramics, there is a case where the collected braided pieces have an adverse effect due to contact with the metal surface.

Therefore, the inventors have further studied and found that, when forming an insulating ceramic coating having a resistivity ρ of 10 ⁵ Ωm or more on at least the tip of the metal needle by a dry plating method, A method for manufacturing a ceramic needle for medical use, wherein a metal needle is set in parallel with the traveling direction of the vapor-deposited particles, and the distal end of the metal needle is placed facing the vapor-deposited particles. (For example, see Patent Document 3).

FIG. 1 schematically shows a magnetron-sputtering type dry plating apparatus disclosed in Patent Document 3. FIG. 2 (a) shows an installation posture of a metal needle as a raw material, and FIG. 2 (b) shows an enlarged cross section of the tip of the metal needle after coating with a ceramic film.
In the figure, reference numeral 1 denotes a vacuum chamber, 2 denotes a sample holder, 3 denotes a metal needle, 4 denotes a ferro-silicon as a target, 5 denotes a magnet, 6 denotes a copper plate interposed therebetween, and 7 denotes a water cooling tube. is there. Further, 8 is a reaction gas inlet, 9 is ionized Si particles, 10 is a jig for fixing the metal needle 3, and 11 and 12 are ceramics formed on the outer and inner surfaces of the metal needle 3, respectively. It is a membrane. The inside of the vacuum chamber 1 is usually kept at a high degree of vacuum of about 0.13 Pa (1 × 10 ⁻³ Torr).

In the place shown in FIG. 1, the ionized Si particles 9 react with a nitrogen gas which is a reaction gas while traveling straight against the metal needle 3 fixed by the sample holder 2, and form SiN _X of the metal needle 3. It will be deposited on the tip.

In this method, when forming the above-mentioned vapor-deposited particles, that is, the SiN _X ceramic, the metal needle 3 is moved in parallel with the traveling direction of the vapor-deposited particles and the vapor-deposited particles that travel along the tip of the metal needle 3. There is a feature in that it is installed to face.
By adopting such an installation posture, the vapor deposition particles effectively penetrate and adhere to the inside of the metal needle 3, and as shown in FIG. 2 (b), not only on the outer surface but also on the inner surface. The insulating ceramic film 12 is effectively covered.

  The development of this technology ensures that the inner surface of the puncture needle is also coated with insulating ceramic, which has no adverse effect on the cells surrounding the puncture needle that stabbed the lesion, as well as on the collected tissue piece itself This makes it possible to obtain a ceramic-coated needle for medical use without any problems.

JP 2003-210579A (Claims) Japanese Patent Application No. 2002-288654 (Claims) Japanese Patent Application No. 2003-9367 (Claims)

However, in the manufacturing method disclosed in Patent Document 3, since the installation position of the metal needle is fixed, coating unevenness such as thick coating on only the tip side of the coating member occurs, or a large number of metals are formed. When coating the needles simultaneously, there is a problem that uneven coating occurs between the metal needles depending on the installation position.
In addition, the above-mentioned manufacturing method is a batch method, and the number of pieces that can be processed by one coating is limited. Therefore, there is a problem that the coating cost is high.

The present invention advantageously solves the above-described problems, and does not fix the installation position of the metal needle, for example, by moving the metal needle up and down, left and right or other directions, thereby coating each ceramic coated needle. It is an object of the present invention to propose a method of manufacturing a ceramic-coated needle that eliminates unevenness and enables an advantageous improvement in coating adhesion, together with a suitable manufacturing apparatus for use in the practice.
Another object of the present invention is to propose a continuous production apparatus for a ceramic-coated needle that can continuously perform ceramic coating on a metal needle as described above.

That is, the gist configuration of the present invention is as follows.
1. At least at the tip of the metal needle, when forming a ceramic coating by a dry plating method,
The metal needle is set in a posture parallel to the traveling direction of the vapor-deposited particles, and in a position where the tip of the metal needle faces the vapor-deposited particles that are traveling. With respect to the traveling direction of the deposited particles, ceramic coating is performed while moving forward and backward, crossing, rotating around the traveling direction as a rotation axis, or revolving with a rotation axis parallel or perpendicular to the traveling direction. A method for producing a ceramic-coated needle.

2. A ceramic coating device for forming a ceramic coating on at least a tip portion of a metal needle, comprising a dry plating device and a sample holder inside a vacuum chamber, wherein the sample holder is a metal to be processed. Move the needle in a direction parallel to the traveling direction of the vapor-deposited particles, and with the tip of the metal needle holding the posture facing the vapor-deposited particles, while moving forward and backward with respect to the traveling direction of the vapor-deposited particles. An apparatus for manufacturing a ceramic-coated needle, comprising: a moving jig that enables movement, rotation with the traveling direction as a rotation axis, or revolving movement with a rotation axis parallel or perpendicular to the traveling direction. .

3. While continuously introducing the sample holder holding the metal needle as the material to be processed into the preliminary chamber for coating, the high vacuum chamber, the ceramic coating chamber, the cooling chamber, and the preliminary chamber after coating, the ceramic coating is performed. A continuous apparatus for producing a ceramic-coated needle for coating a ceramic coating on the tip of the metal needle in a chamber, wherein a dry plating apparatus is disposed in the ceramic coating chamber, and the sample holder is disposed in the ceramic coating chamber. The metal needle that is the material to be processed is moved in the direction in which the vapor-deposited particles travel in a direction parallel to the direction in which the vapor-deposited particles travel, and while maintaining a posture in which the tip of the metal needle faces the vapor-deposited particles. On the other hand, forward / backward movement, crossing movement, rotation movement with the traveling direction as a rotation axis, or rotation axis parallel or perpendicular to the traveling direction Continuous apparatus for producing a ceramic-coated needle characterized by comprising a moving jig makes it possible to publicly rotation movement to.

ADVANTAGE OF THE INVENTION According to this invention, the coating of a ceramic film can be obtained, and the ceramic-coated needle excellent in film adhesion can be obtained.
Further, according to the present invention, it is possible to continuously obtain the above-mentioned ceramic-coated needle having no coating unevenness and excellent in film adhesion, so that an improvement in productivity and a reduction in cost can be achieved.

Hereinafter, the present invention will be specifically described with reference to the drawings.
FIG. 3 schematically shows a preferred example of a magnetron sputtering type dry plating apparatus according to the present invention. The outline of the configuration is the same as that of the conventional apparatus shown in FIG. 1 and is therefore denoted by the same reference numeral, and reference numeral 13 is a movable sample holder. In this example, the movable sample holder 13 is of a cart type as shown in FIG. 4, and has a mechanism capable of horizontal movement, that is, cross movement with respect to the traveling direction of vapor deposition particles. In the figure, reference numeral 14 denotes a mobile trolley, and 15 denotes a sample trolley.

  As described above, the coating is performed while the sample holder 13 is cross-moved as indicated by the symbol A, so that the deposited particles can be removed from the outer surface of the metal needle without increasing the adhesion amount only on the tip side. Not only that, but also the inner surface adhered uniformly, and as a result, the occurrence of uneven coating, which had been a concern in the past, was effectively eliminated.

In addition, by adopting such a moving method, the adhesion of the ceramic coating was improved.
The reason for this is that, in general, in the fixed type coating, the epitaxial growth of the deposited particles takes precedence, so that the coating unevenness is promoted, whereas in the mobile type coating like the present invention, such a phenomenon does not occur. It is considered that the adhesion of the ceramic coating was improved.

  Further, in the present invention, the movement of the sample holder is not limited to the cross movement with respect to the traveling direction of the vapor deposition particles, but moves forward and backward with respect to the traveling direction of the vapor deposition particles as shown by symbols B and C in FIG. Alternatively, it may be a rotational movement having the traveling direction as a rotation axis.

Further, the movement of the sample holder may be a revolving movement having a rotation axis parallel or perpendicular to the traveling direction of the deposition particles.
FIG. 5 schematically shows a vertical revolving jig having parallel rotation axes and capable of revolving. In this case, since the large turntable 16 rotates (revolves) and the small turntable 17 also rotates (rotates) at the same time, the metal needles 3 installed in the sample holder are evenly distributed in the vacuum chamber 1. Therefore, the occurrence of uneven coating can be prevented more effectively.

  FIG. 6 schematically shows a horizontal revolving jig having a vertical rotation axis and capable of revolving. In this case, the small disk 19 is rotated (rotated) in synchronization with the rotation (revolution) of the large disk 18 so that the metal needle 3 installed on the sample holder 13 can always maintain a vertical posture. is important. According to this method, as in the case of FIG. 5, the occurrence of uneven coating can be effectively prevented.

  Furthermore, in the above-described apparatus, since a large number of metal needles can be set on a plurality of movable carts and the coating process can be performed simultaneously, there is an advantage that productivity is improved and cost is significantly reduced.

  Although various movement modes have been described above, the present invention is not limited to this. In short, the installation position of the metal needle is not fixed, and the installation posture of the metal needle is always in the traveling direction of the deposition particles. Any other movement form may be used as long as the posture is kept parallel to and at a position facing the vapor deposition particles. The above-described movement may be continuous or may be intermittent.

In the above example, the case where the ceramic coating is performed in a batch manner has been mainly described. However, in the present invention, the ceramic coating on the metal needles can be continuously performed in a continuous coating line.
Hereinafter, a continuous manufacturing apparatus that enables the above-described continuous coating will be described.

FIG. 7 schematically shows an apparatus for continuously manufacturing ceramic-coated needles according to the present invention, wherein reference numeral 20 denotes a preliminary chamber for coating, 21 denotes a high vacuum chamber, 22 denotes a ceramic coating chamber, 23 denotes a cooling chamber, and 24 denotes a coating. A later spare room, and 25 is a trajectory for moving the sample holder 13.
In the present invention, the sample holder 13 holding the metal needle 3 as a material to be processed is sequentially guided along the track 25 into these chambers 20 to 24, and in the meantime, in the ceramic coating chamber 22, the metal holder 3 is moved relative to the metal needle 3. Ceramic coating by dry plating.
In addition, although illustration is omitted, each chamber is partitioned by a partition, and the partition can be opened and closed as needed.

Here, the coating preparatory chamber 20 is a chamber for pre-evacuating the metal needle, and is usually kept at a low vacuum of about 1.33 Pa (1 × 10 ^-2 Torr).
The high vacuum chamber 21 is a chamber for cleaning the surface of the metal needle or removing gas adsorbed on the surface of the metal needle, and is usually 6.7 × 10 ⁻³ Pa (5 × 10 ⁻⁵ Torr). It is kept at a high degree of vacuum.

Further, in the ceramic coating chamber 22, as shown in FIG. 3, the ceramic coating is performed while the sample holder 13 holding the metal needle 3 is moved (crossed) on the track 25.
In this continuous manufacturing apparatus, the movement of the sample holder 13 in the traveling direction of the vapor deposition particles is most efficiently performed by cross movement as indicated by the symbol A in FIG. 3, but if necessary, a special jig may be used. It is needless to say that a reciprocating movement and a rotational movement as shown by symbols B and C in FIG. 4 and a revolving movement as shown in FIGS. 5 and 6 may be provided.
The ceramic coating chamber 22 is usually maintained at a high vacuum of about 0.13 Pa (1 × 10 ⁻³ Torr).

Next, the cooling chamber 23 is a chamber for lowering the temperature of the metal needle 3 raised to about 300 ° C. to about 50 to 60 ° C. by the coating treatment in the ceramic coating chamber 22. The temperature is maintained at about 0.13 to 1.33 Pa (1 × 10 ⁻³ to 1 × 10 ⁻² Torr).
The prechamber 24 after coating is a chamber for preliminarily cooling the coated ceramic needles, and is usually kept at a vacuum degree of about 0.67 Pa (5 × 10 ⁻³ Torr).

When the above-mentioned metal needle is used as a puncture needle, the outer surface of the puncture needle is not necessarily required to be coated with the ceramic coating on the entire surface of the needle. It would be fine.
In this regard, the same applies to the inner surface of the puncture needle, as long as it is covered with the ceramic film by at least 1 mm from the base to the inside of the inclined region at the tip of the needle (the region indicated by h in FIG. 2B). . The reason for this is that if the inner surface of the puncture needle is not covered with the insulating ceramic film over at least 1 mm, the collected tissue piece may be adversely affected. Preferably, the ceramic film is preferably coated on the inside of the needle tip about 3 to 10 mm from the base.

When used for gene control, at least a portion of the outer surface that contacts a living tissue, and at least a portion of the inner surface that contacts a cell nucleus in the living tissue are sufficient.
Specifically, the outer surface is at least 1 mm, preferably at least 10 mm from the tip of the metal needle, while the inner surface is at least 10 μm, preferably at least 1 mm from the tip of the metal needle.

Further, in the present invention, since a ceramic coating is formed on the surface of the needle, any material can be used as the base material of the needle, as long as it is a metal material. Particularly preferred is an iron such as stainless steel or high-tensile steel. It is a base metal.
This is because iron-based metals are extremely easy to perform precision processing, and stainless steel also has the advantage that the surface does not rust. Among these stainless steels, ferritic stainless steels are particularly advantageously suited.

  For example, when manufacturing a base for a puncture needle from stainless steel, the stainless steel material is continuously cast, hot-rolled, cold-rolled, bright-annealed, and then precision-processed to an outer diameter of 0.5 to 2.5 mm, length. Sa: It is processed into various needle shapes according to the purpose of about 100 to 250 mm. Note that the processing steps at this time may be performed according to a conventional technique.

Next, after the surface of the obtained needle is cleaned by ultrasonic cleaning, electrolytic polishing, or the like, a ceramic coating is formed as described above. It is important to use an insulating ceramic of 10 ⁵ Ω · m or more. This is because a ceramic having a resistivity ρ of less than 10 ⁵ Ω · m cannot completely wipe out the adverse effects on the cells around the collected tissue piece and the puncture needle pierced into the lesion.
As such an insulating ceramic, SiO ₂ , BN, Al ₂ O _3, etc., besides SiN _X described above are advantageously adapted.

Further, the ceramic coating as described above is applied by a dry plating method. As such a dry plating method, a magnetron sputtering method capable of high ionization and high-speed film formation is optimally applied, but other known methods such as RF (Radio Frequency), hollow cathode discharge method, and arc discharge method are used. A PVD coating method, a CVD coating method or a high plasma CVD coating method can also be used.
Here, the preferable coating conditions of the ceramic coating by the magnetron sputtering method are as follows.
For example, when a ferrosilicon target is used to perform SiN _X coating, the input power is 5 to 10 kW, the degree of vacuum is 1.06 × 10 ^{−2 to} 3.99 × 10 ⁻¹ Pa (0.8 × 10 ^{−4 to} 3). (× 10 ⁻³ Torr), Ar gas: 50 to 1000 sccm, and N ₂ gas: 50 to 1000 sccm are optimal conditions.

In addition, during the above-mentioned plasma coating, particularly in the latter half thereof, by introducing O ₂ at about 5 to 500 sccm, it is possible to coat an extremely insulating ceramic coating having a resistivity ρ of 10 ⁹ Ωm or more. .

C: 0.027 mass%, Si: 0.3 mass%, Mn: 0.18 mass%, P: 0.012 mass%, S: 0.009 mass%, and Cr: 18.2 mass%, with the balance being Fe and unavoidable impurities A ferritic stainless steel material was continuously cast, subjected to hot rolling-cold rolling-bright annealing, and then precision-worked to produce a metal needle having an outer diameter of 0.8 mm and a length of 200 mm. Then, after ultrasonic cleaning, a SiN _x film was formed in a high plasma atmosphere using the magnetron sputtering apparatus shown in FIG.
In forming the SiN _x ceramic film by the magnetron sputtering method, the film was formed to a thickness of 1.0 μm in Ar: 500 sccm and N ₂ : 200 sccm. The coating area of the SiN _x ceramic film was 60 mm from the tip of the needle on the outer surface, and 7 mm from the tip of the needle (root of the opening) on the inner surface.
For comparison, a ceramic-coated needle was prepared using the apparatus shown in FIG. 1 under the same conditions as in the example.

The coating unevenness and coating adhesion of the ceramic-coated needle thus obtained were examined.
Here, the coating unevenness was evaluated by the difference in coating thickness (μm) between the tip of the ceramic-coated needle and the inner surface 5 mm from the tip. The coating thickness was determined by observing the coating cross section with a scanning electron microscope.
Furthermore, the coating adhesion was evaluated at the minimum diameter at which the ceramic coated steel sheet having a ceramic film formed on the surface of a separately prepared stainless steel sheet by a similar method was not peeled even when bent 180 °.

  As is evident from the table, the ceramic-coated needle obtained according to the present invention had significantly improved coating unevenness and good film adhesion as compared with the comparative example.

FIG. 2 is a schematic diagram of a dry plating apparatus (magnetron sputtering method) in which a sample holder is fixed. (a) is a diagram showing an installation mode of a metal needle with respect to a sample holder, and (b) is an enlarged cross-sectional view of a tip portion of the metal needle. FIG. 1 is a schematic view of a magnetron-sputtering type dry plating apparatus suitable for use in manufacturing the ceramic-coated needle of the present invention. It is a detailed view of a sample holder. FIG. 3 is a schematic view of a vertical revolving jig capable of revolving and having a rotation axis parallel to a traveling direction of vapor deposition particles. It is a schematic diagram of a horizontal revolving jig which can be revolved and has a rotation axis perpendicular to the traveling direction of vapor deposition particles. 1 is a schematic view of an apparatus for continuously manufacturing a ceramic-coated needle according to the present invention.

Explanation of reference numerals

DESCRIPTION OF SYMBOLS 1 Vacuum tank 2 Sample holder 3 Metal needle 4 Ferrosilicon target 5 Magnet 6 Copper plate 7 Water cooling tube 8 Reaction gas inlet 9 Ionized Si particles
10 Metal needle fixing jig
11 Ceramic film formed on outer surface of metal needle
12 Ceramic film formed on the inner surface of metal needle
13 Mobile sample holder
14 Moving trolley
15 Sample stand
16 large turntable
17 Small turntable
18 large disk
19 small disk
20 Coating spare room
21 High vacuum chamber
22 Ceramic coating room
23 Cooling room
24 Spare room after coating
25 orbits

Claims (3)

At least at the tip of the metal needle, when forming a ceramic coating by a dry plating method,
The metal needle is set in a posture parallel to the traveling direction of the vapor-deposited particles, and in a position where the tip of the metal needle faces the vapor-deposited particles that are traveling. With respect to the traveling direction of the deposited particles, ceramic coating is performed while moving forward and backward, crossing, rotating around the traveling direction as a rotation axis, or revolving with a rotation axis parallel or perpendicular to the traveling direction. A method for producing a ceramic-coated needle.   A ceramic coating device for forming a ceramic coating on at least a tip portion of a metal needle, comprising a dry plating device and a sample holder inside a vacuum chamber, wherein the sample holder is a metal to be processed. Move the needle in a direction parallel to the traveling direction of the vapor-deposited particles, and with the tip of the metal needle holding the posture facing the vapor-deposited particles, while moving forward and backward with respect to the traveling direction of the vapor-deposited particles. An apparatus for manufacturing a ceramic-coated needle, comprising: a moving jig that enables movement, rotation with the traveling direction as a rotation axis, or revolving movement with a rotation axis parallel or perpendicular to the traveling direction. .   While continuously introducing the sample holder holding the metal needle as the material to be processed into the preliminary chamber for coating, the high vacuum chamber, the ceramic coating chamber, the cooling chamber, and the preliminary chamber after coating, the ceramic coating is performed. A continuous apparatus for producing a ceramic-coated needle for coating a ceramic coating on the tip of the metal needle in a chamber, wherein a dry plating apparatus is disposed in the ceramic coating chamber, and the sample holder is disposed in the ceramic coating chamber. The metal needle that is the material to be processed is moved in the direction in which the vapor-deposited particles travel in a direction parallel to the direction in which the vapor-deposited particles travel, and while maintaining a posture in which the tip of the metal needle faces the vapor-deposited particles. On the other hand, forward / backward movement, crossing movement, rotation movement with the traveling direction as a rotation axis, or rotation axis parallel or perpendicular to the traveling direction Continuous apparatus for producing a ceramic-coated needle characterized by comprising a moving jig makes it possible to publicly rotation movement to.

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