JP2002243594A - Sampling jig and infrared spectrometric method using it - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a sampling jig capable of easily and surely implementing the composition analysis of a minute sample, and an infrared spectrometric method using it. SOLUTION: In this sampling jig for collecting the minute sample in infrared spectrometry, an adhesive material of a prescribed thickness is applied to a sampling part for adhering the sample on the tip side of the jig, so that the sample can be set in a prescribed position in the adhered state and irradiated with spectrometric infrared rays.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a jig for sampling a minute sample at the time of infrared spectroscopy measurement and an infrared spectroscopy method using the same.

[0002]

2. Description of the Related Art As is well known, in the manufacture of a product, a minute foreign matter may be mixed into the product during the manufacturing process or during transportation or leaving between each process, which may cause a failure of the product. Therefore, by preventing the entry of minute foreign matter, the yield of products is improved, and the reliability and manufacturing efficiency of the products can be improved. As a countermeasure for preventing such foreign matter, conventionally, for example, foreign matter actually mixed into a product, such as an organic substance attached to a glass substrate constituting a TFT panel, is collected, the composition thereof is analyzed, and based on the result thereof, Elimination of foreign matter sources has been performed.

[0003] As a method of collecting foreign matter in the composition analysis of a minute foreign matter, for example, a method using a micro-infrared measuring apparatus which is a kind of infrared spectroscopy is known. In this method, a micro sample having a size of several μm to several mm is attached to a pointed tip of a needle with a natural electrostatic force and adhesive force of the sample under a stereoscopic microscope. Potassium bromide (KB
r) A small sample is transferred onto a substrate such as a crystal plate that transmits infrared light, and the substrate is placed on a sample table of a micro-infrared measuring device for analysis.

As a method of collecting foreign matter when analyzing the composition of a minute foreign matter, see, for example, Japanese Patent Laid-Open No. 5-20838.
As disclosed in Japanese Unexamined Patent Publication No. 7-1995, a sampling method using a manipulator is known. FIG. 8 schematically shows the configuration of the manipulator. 53b is a metal capillary,
55 shows a sample. Numeral 58 indicates a DC power source, and numeral 59 indicates a changeover switch for switching voltage polarity. First, a voltage of, for example, +1200 V is applied to the tip of the metal capillary 53 b using the DC power supply 58, and the metal capillary 53 b is brought closer to the sample 55. At this time, the sample 55 is adsorbed on the tip of the metal capillary 53b by the action of static electricity and collected. When it comes to a predetermined position on the measurement substrate or the like, the changeover switch 59 causes the metal capillary 53b to be depressed by -1.
The sample 55 is dropped by switching to the reverse polarity of 200V. Then, the substrate is placed on a sample stage and analyzed.

[0005]

However, in the former method, the attachment of the sample to the needle tip is performed by the natural electrostatic force and adhesive force of the sample, so that the minute sample can be as large as several hundred μm or more. Then, the weight of the sample becomes larger than the electrostatic force and the adhesive force of the sample. Therefore, when a sample is collected or transferred onto a measurement substrate, the sample often falls off the needle tip and is lost, which is not reliable. Conversely, a sample as small as a few μm has a greater electrostatic force and adhesive force than its own weight, and does not easily separate when transferring from the sampled needle tip onto the measurement substrate, making it difficult and difficult to work. There is a problem that requires.

On the other hand, in the latter method, a metal capillary 5 is used.
The attachment of the sample to 3b requires equipment such as a power supply and is not simple. In this case, although the sample can be moved relatively easily, it is necessary to transfer the sample onto the measurement substrate in order to perform the composition analysis, as in the former method.

SUMMARY OF THE INVENTION The present invention has been made in view of the above technical problems, and a sampling jig capable of easily and reliably realizing composition analysis of a minute sample and an infrared spectroscopy method using the same. The purpose is to provide.

[0008]

According to a first aspect of the present invention, there is provided a sampling jig for collecting a small sample at the time of infrared spectroscopic measurement. Adhesive substance is applied,
The apparatus is characterized in that it is installed at a predetermined position in a state where the sample is attached, and can be irradiated with infrared light for spectral measurement.

According to a second aspect of the present invention, in the first aspect, the sampling portion on the tip side of the jig is made of a metal material having infrared light reflectivity of a predetermined level or more. is there.

Further, according to a third invention of the present application, in the first invention, the sampling portion on the tip end side of the jig is made of a material that transmits infrared light and has an infrared light absorbing property equal to or less than a predetermined value. It is characterized by.

[0011] Further, the fourth invention of the present application is the first invention.
In any one of the third inventions, the adhesive substance may be 2
The coating is characterized by being applied with a uniform film thickness in the range of 0 nm to 100 nm.

[0012] Further, the fifth invention of the present application is the first invention.
3. The method according to claim 1, wherein the pressure-sensitive adhesive substance has an infrared light absorption of not more than a predetermined value, and is applied with a uniform film thickness in a range of 100 nm to 2 μm. is there.

Further, the sixth invention of the present application provides
5. An infrared spectroscopic measurement method using the sampling jig according to any one of the fifth aspect of the invention, wherein the sampling jig is set at a predetermined position in a state where a sample is attached to a sampling portion on a tip side thereof. The above is characterized in that infrared light for spectral measurement is irradiated to perform infrared spectral measurement.

[0014]

Embodiments of the present invention will be described below with reference to the accompanying drawings. Embodiment 1 FIG. (A) and (b) of FIG.
It is a top view and a longitudinal section explanatory view schematically showing a sampling jig according to Embodiment 1 of the present invention. The sampling jig 10 is formed in a rod shape as a whole, and collects a sample on the tip side thereof, and is installed at a predetermined position with the sample attached thereto, and can be irradiated with infrared light for spectral measurement. It is configured as follows. In the following description, a sample having a size of several μm to several mm is an object of the composition analysis.

The sampling jig 10 has a sampling section 2 for collecting a sample at a tip end thereof, and a grip section 3 for an operator to hold the jig. The sampling unit 2 is formed in a flat plate shape.
It is made of a metal material such as stainless steel having infrared light reflectivity higher than a predetermined value. Aluminum and stainless steel are relatively inexpensive and hard to rust, have excellent durability, and are easy to process. In particular, aluminum has the advantage that the reflectance of infrared light is large and easy to measure, while stainless steel is hard and easy to sample. Note that the metal material forming the sampling unit 2 is not limited to these, but may be any material that reflects infrared light.

An adhesive film is applied on the sampling section 2 and has a predetermined thickness (1 μm in this embodiment).
Are formed. Generally, as the thickness of the adhesive film 5 increases, the light absorption by the adhesive film 5 increases,
When irradiating infrared light to the above sample to analyze its composition, it may affect measurement data as noise.
In order to avoid this, as an adhesive film constituting the adhesive film 5,
For example, those having a predetermined or lower infrared light absorption such as a hydrocarbon-based adhesive film such as isoprene and nujol, a silicon-based adhesive film, and a fluorine-based adhesive film such as KRYTOX manufactured by DuPont are used. The adhesive film constituting the adhesive film 5 includes:
The material is not limited to these, and any material may be employed as long as it has a viscosity to which the micro sample adheres and has an infrared light absorption of a predetermined value or less. In the present invention, the term “infrared light absorbing property” corresponds to the spread of the wavelength absorbed by a substance. That is, the substance having an infrared light absorption of a predetermined value or less refers to a substance whose absorption wavelength can be suppressed to a predetermined width or less. The substance can also be treated as having a predetermined or lower infrared light absorption.

Adhesive film 5 formed on sampling section 2
Is set in the range of 100 nm to 2 μm,
As the adhesive film constituting the adhesive film 5, a film having an infrared light absorption of a predetermined value or less is used. When the thickness of the adhesive film 5 is further reduced, for example, in the range of 20 nm to 100 nm, if the material has a viscosity to which the sample adheres,
The substance may not be a substance having low infrared light absorption. This is because the intensity of the absorption peak based on the adhesive film 5 is sufficiently small so as not to cause noise in the measurement data, in view of the detection sensitivity of infrared spectrometry.

As a method of forming the adhesive film 5 having a uniform thickness on the sampling unit 2, a method of immersing the sampling unit 2 of the jig 10 in, for example, an adhesive substance solution diluted with a solvent and drying the solvent is used. Adopted. The method for forming the adhesive film 5 is not limited to this. For example, a method in which an adhesive substance solution diluted with a solvent is applied on the sampling unit 2 by a spin coating method and the solvent is dried may be used. Good. In such a method, if the sampling unit 2 can be detached from the grip unit 3, spin coating can be performed more easily.

An infrared spectroscopic measurement method using the sampling jig 10 having the above-described configuration will be described. FIG.
FIG. 4 is an explanatory diagram of an infrared spectroscopic measurement method. At the time of infrared spectroscopy measurement, the sample 6
The sampling jig 10 to which the sample 6 is attached irradiates the sample 6 with the incident light P of the infrared light emitted from the light source 7 and the reflected light Q reflected by the sampling unit 2
It is positioned so that it is guided to. Here, a Fourier transform infrared spectrometer is used as the infrared spectrometer, and in this device, a glow bar light source and a detector 9 are used as the light source 7.
, A high-sensitivity MCT detector is used.

In the infrared spectroscopy, first, the sample 6 is measured to obtain the spectrum of the sample 6. Next, the adhesive film 5
The same measurement is performed on a portion of the sampling unit 2 where the sample 6 does not adhere to the sample, and this data is used as a measurement reference. In this case, the thickness of the adhesive film 5 is uniform, and the peak intensity of the adhesive film 5 is almost the same between the portion where the sample 6 is present and the portion where the sample 6 is not present. The subtraction can be easily performed, and the influence of the adhesive film 5 can be minimized.

As described above, according to the sampling jig 10, the adhesive film 5 for attaching the sample to the sampling section 2 is used.
Is formed, and the adhesive force of the sample and the adhesive film 5 acts on each other to increase the adhesive force relatively. Therefore, it is possible to sufficiently prevent the sample from falling off from the sampling unit 2.
Further, since the sampling unit 2 is made of a measurable material, the infrared spectroscopy measurement can be performed on the sample adhered by the sampling unit 2 without transferring the sample to the measurement substrate. The composition analysis of a sample can be performed easily and reliably. Furthermore, the sampling jig 10 is relatively simple in construction and can be used easily.

FIGS. 3, 4 and 5 show modifications of the sampling jig 10 according to the first embodiment, respectively.
In the sampling jig according to these modified examples, each sampling unit is formed in a different shape from the sampling unit 2 (see FIG. 1) according to the first embodiment. FIG.
4A and 4B are formed in a knife shape, and the sampling portions 12 shown in FIGS. 4A and 4B are formed in a triangular shape. When these sampling units 11 and 12 are used, a minute sample can be easily peeled off from the adhering surface at a sharp portion or a sharp portion.

Further, the sampling section 13 shown in FIGS. 5A and 5B includes a reflection plane area 13a and the plane area 1a.
And a taper region 13b formed in a tapered shape toward the distal end side adjacent to 3a. When this is used, the minute foreign matter can be peeled off by the sharp taper region 13b. Since the reflection plane region 13a is relatively wide, infrared spectroscopy can be easily performed.

Embodiment 2 FIG. FIG. 6 is a sectional explanatory view schematically showing a sampling jig 20 according to Embodiment 3 of the present invention. The sampling jig 20 has a flat sampling part 22 and a cylindrical holding part 23 which is formed in a cylindrical shape and which is fitted into an opening at one end of the sampling part 22. The sampling unit 22 is made of a material that transmits infrared light and has an infrared light absorbability of a predetermined value or less. As the material of the sampling unit 22, for example, germanium, silicon, potassium bromide, sodium chloride, thallium bromide-thallium iodide (KRS-5) can be used. In particular, germanium and silicon are hard and easy to sample, sodium chloride is excellent in permeability and inexpensive, and thallium bromide-thallium iodide (KRS-5) has the advantage of being resistant to water. . The material of the sampling section 22 is not limited to these, and any material may be used as long as it transmits infrared light and has low infrared light absorption.

An adhesive film 25 having a uniform thickness is formed on the surface exposed outside the sampling section 22. This adhesive film 25 is formed in the same manner as the adhesive film 5 according to the first embodiment. In the sampling jig 20, the sample is adhered and collected by pressing the sample portion 22 on which the adhesive film 25 is formed against the sample to be analyzed.

FIG. 7 is an explanatory diagram of an infrared spectroscopic measurement method using the sampling jig 20. At the time of infrared spectroscopy measurement, the sample 6 is placed on the adhesive film 25 on the sampling unit 22.
Is attached to the sample 6 and the sample 6 is irradiated with the incident light R of the infrared light emitted from the light source 7, and the transmitted light S transmitted through the sampling unit 22 is detected by the detector 9.
Is positioned to be guided to Here, a Fourier transform infrared spectrometer is used as the infrared spectrometer, and in this device, a glow light source and a detector 9 are used as the light source 7.
, A high-sensitivity MCT detector is used. As can be seen from FIG. 7, the sampling jig 20 is disposed between the light source 7 and the detector 9 in a state where it is positioned, and the light from the light source 9 has transmitted through the sampling unit 22. Thereafter, the light passes through the inside of the cylindrical holding portion 23 and enters the detector 9.

In this infrared spectroscopic measurement, the first embodiment is used.
First, the measurement of the sample 6 is performed, and the spectrum of the sample 6 is obtained, as in the case of. Next, the same measurement is performed on a portion of the sampling unit 22 where the adhesive film 25 is present and to which the sample 6 is not attached, and this data is used as a measurement reference. In this case, the thickness of the adhesive film 25 is uniform, and the peak intensity of the adhesive film 25 is almost the same between the portion where the sample 6 is present and the portion where the sample 6 is not present.
The absorption peak of the adhesive film 25 can be easily subtracted, and the influence of the adhesive film 25 can be minimized.

As described above, according to the sampling jig 20, the adhesive film 25 for attaching the sample is formed on the sampling section 22, and the adhesive force of the sample and the adhesive film 25 acts on each other, so that the adhesive force is relatively small. Since the size becomes large, it is possible to sufficiently prevent the sample from dropping out of the sampling unit 2. In addition, since the sampling unit 22 is made of a measurable material, it is possible to perform infrared spectroscopy measurement on the sample adhered by the sampling unit 22 without transferring the sample to the measurement substrate. The composition analysis of a sample can be performed easily and reliably. Furthermore, the sampling jig 20 is configured relatively simply,
Easy to use.

The present invention is not limited to the illustrated embodiment, and it goes without saying that various improvements and design changes can be made without departing from the spirit of the present invention.

[0030]

According to the invention of claim 1 of the present application, in a sampling jig for collecting a small sample at the time of infrared spectroscopic measurement, an adhesive having a predetermined thickness is attached to a sampling portion on a tip side of the jig to which the sample is attached. Since the adhesive is applied to the sample, the sample is attached to the predetermined position in a state where the sample is attached, and is configured to be able to irradiate infrared light for spectroscopic measurement. When applied, the adhesive force is relatively large, and the sample can be sufficiently prevented from dropping from the sampling section. In addition, even if the sample is not transferred to the measurement substrate, the infrared spectroscopy measurement can be performed on the sample attached at the sampling unit as it is, and the composition analysis of the sample can be easily and reliably performed. it can.

Further, according to the invention of claim 2 of the present application, since the sampling portion on the tip side of the jig is made of a metal material having infrared light reflectivity of a predetermined level or more, the sample attached to the sampling portion can be removed. On the other hand, infrared spectrometry can be performed as it is, and composition analysis of the sample can be easily performed.

Further, according to the invention of claim 3 of the present application, the sampling section on the tip side of the jig transmits infrared light,
Since the sample is made of a material having an infrared light absorbing property equal to or less than a predetermined value, it is possible to directly perform infrared spectroscopy measurement on the sample adhered in the sampling section, and it is possible to easily perform composition analysis of the sample.

Further, according to the invention of claim 4 of the present application, since the adhesive substance is applied in a uniform film thickness in the range of 20 nm to 100 nm, the absorption peak based on the adhesive substance is reduced. The intensity can be made sufficiently small so as not to cause noise in the measurement data, and the infrared spectroscopic measurement can be satisfactorily performed on the sample adhered in the sampling section.

Further, according to the invention of claim 5 of the present application, the above-mentioned adhesive substance has an infrared light absorption of not more than a predetermined value and is applied with a uniform film thickness in the range of 100 nm to 2 μm. As a result, the intensity of the absorption peak based on the adhesive substance can be made sufficiently small so as not to cause noise in the measurement data, and the infrared spectroscopic measurement is performed satisfactorily on the sample adhered in the sampling unit. be able to.

According to a sixth aspect of the present invention, there is provided an infrared spectroscopic measurement method using the sampling jig according to any one of the first to fifth aspects of the present invention. The jig is placed at a predetermined position with the sample attached to its tip, and then irradiated with infrared light for spectroscopic measurement to perform infrared spectroscopic measurement. Act on each other to have a relatively large adhesive force, and it is possible to sufficiently prevent the sample from falling off the sampling section. In addition, even if the sample is not transferred to the measurement substrate, the infrared spectroscopy measurement can be performed on the sample attached at the sampling unit as it is, and the composition analysis of the sample can be easily and reliably performed. it can.

[Brief description of the drawings]

FIG. 1A is a plan view showing a sampling jig according to Embodiment 1 of the present invention. (B) It is a longitudinal section explanatory view showing the above-mentioned sampling jig.

FIG. 2 is an explanatory diagram of an infrared spectroscopic measurement method using the sampling jig.

FIG. 3A is a plan view showing a first modification of the sampling jig according to the first embodiment. (B) It is a longitudinal section explanatory view showing the above-mentioned 1st modification.

FIG. 4A is a plan view showing a second modification of the sampling jig according to the first embodiment. (B) It is a longitudinal section explanatory view showing the second modification.

FIG. 5A is a plan view showing a third modification of the sampling jig according to the first embodiment. (B) It is a longitudinal section explanatory view showing the above-mentioned third modification.

FIG. 6 is an explanatory sectional view showing a sampling jig according to a second embodiment of the present invention.

FIG. 7 is an explanatory diagram of an infrared spectroscopic measurement method using the sampling jig according to the second embodiment.

FIG. 8 is a schematic view of a conventionally known manipulator.

[Explanation of symbols]

2,22 sampling part, 3,23 gripping part, 5,2
5 adhesive film, 6 sample, 7 light source, 9 detector, 10,
20 Sampling jig, P, R incident light, Q reflected light, S transmitted light

 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 2G052 AA00 AA40 AC23 AD12 AD52 BA23 DA05 DA21 GA11 JA04 JA08 JA15 2G059 AA01 BB08 CC01 DD12 EE01 EE02 EE10 EE12 FF08 GG10 HH01 KK01

Claims (6)

[Claims] 1. A sampling jig for collecting a small sample at the time of infrared spectroscopy measurement, wherein:
A sampling jig, which is provided with a predetermined thickness of an adhesive substance, is set at a predetermined position with the sample attached thereto, and is configured to be irradiated with infrared light for spectral measurement. Utensils. 2. The sampling jig according to claim 1, wherein the sampling portion on the tip side of the jig is made of a metal material having infrared light reflectivity of a predetermined level or more. 3. The sampling jig according to claim 1, wherein the sampling portion on the front end side of the jig is made of a material that transmits infrared light and has an infrared light absorbing property equal to or less than a predetermined value. 4. The method according to claim 1, wherein the adhesive substance has a thickness of 20 nm to 100 n.
The sampling jig according to claim 1, wherein the jig is applied with a uniform film thickness in a range of m. 5. The method according to claim 1, wherein the pressure-sensitive adhesive substance has an infrared light absorption of not more than a predetermined value and is applied with a uniform film thickness in a range of 100 nm to 2 μm. The sampling jig according to any one of the above. 6. An infrared spectroscopic measurement method using the sampling jig according to claim 1, wherein a sample adheres to a sampling portion on a tip side of the sampling jig. An infrared spectroscopy method characterized by irradiating infrared light for spectrometry after being set at a predetermined position in a state and performing infrared spectroscopy.