Composite structure, semiconductor manufacturing apparatus and display manufacturing apparatus provided with composite structure

Patent metadata

Field	Value
Publication number	US-10759710-B2
Application number	US-201916296934-A
Country	US
Kind code	B2
Filing date	Mar 8, 2019
Priority date	Mar 8, 2018
Publication date	Sep 1, 2020
Grant date	Sep 1, 2020

Abstract

Disclosed is provision of a ceramic coat having an excellent low-particle generation as well as a method for assessing the low-particle generation of the ceramic coat. A composite structure including a substrate and a structure which is formed on the substrate and has a surface, wherein the structure includes a polycrystalline ceramic and the composite structure has luminance Sa satisfying a specific value calculated from a TEM image analysis thereof, can be suitably used as an inner member of a semiconductor manufacturing apparatus required to have a low-particle generation.

First claim

What is claimed is:

1. A composite structure which is in low-particle generation and is used under an environment in which low-particle generation is required, comprising a substrate and a structure provided on the substrate and having a surface; wherein
the structure comprises a polycrystalline ceramic; and
a hydrogen atom number per unit volume of the structure at a measurement depth of either 500 nm or 2 μm is 7×10 21 atoms/cm 3 or less, wherein the hydrogen atom number is measured by a dynamic-secondary ion mass spectrometry (D-SIMS method),
wherein the D-SIMS method is conducted under the following condition that:
conductive platinum (Pt) is vapor-deposited onto the structure surface, a cesium (Cs) ion is used as a primary ion species, a primary acceleration voltage is made to 15.0 kV, and a detection area is made to 8 μmϕ, and wherein a sample which is the same as the structure surface and a Si single crystal are provided as standard samples, and heavy hydrogen are introduce into these standard samples, and it is presumed that the same amount of the heavy hydrogen is introduced into the standard samples, the standard samples are compared with the structure surface and a Si single crystal into which heavy hydrogen is not introduced, thereby a relative sensitivity factor is calculated, and then by using the relative factor, the hydrogen amount of the structure surface is calculated.

2. The composite structure according to claim 1 , wherein the hydrogen atom number per unit volume of the structure is 5×10 21 atoms/cm 3 or less.

3. A composite structure which is in low-particle generation and is used under an environment in which low-particle generation is required, comprising a substrate and a structure provided on the substrate and having a surface; wherein
the structure comprises a polycrystalline ceramic; and
a luminance Sa of the structure is 19 or less, wherein
the luminance Sa is calculated by a method comprising the steps of:
(i) preparing a transmission electron microscope observation samples of the structure,
(ii) preparing a digital white and black image of a bright-field image of each of the transmission electron microscope observation samples,
(iii) obtaining a luminance value expressed by 256 gradations in color data of each pixel in the digital white and black image,
(iv) correcting the luminance value, and
(v) calculating the luminance Sa by using the corrected luminance value; and
in the step (i),
as the transmission electron microscope observation samples, at least three samples are prepared from the structure,
each of the at least three transmission electron microscope observation samples is prepared by using a focused ion beam method with suppressing a processing damage,
during the focused ion beam method, a carbon layer and a tungsten layer are formed on the surface of the structure for prevention of static charge and for sample protection, and
when a direction of the focused ion beam method is taken as a vertical direction, an upper part thickness of each of the samples is 100±30 nm, wherein the upper part thickness of each of the samples is a length of a short axis direction of the surface of the structure in a plane perpendicular to the vertical direction; and
in the step (ii),
the digital white and black image is obtained in each of the at least three transmission electron microscope observation samples,
each of the digital white and black images is obtained by using a transmission electron microscope with a magnification of 100,000 and an acceleration voltage of 200 kV, and includes regions of the structure, the carbon layer, and the tungsten layer,
a luminance-obtaining region is set for each of the digital white and black images, wherein the luminance-obtaining region has a region's vertical length of 0.5 μm in the vertical direction from the surface of the structure, and
each of the digital white and black images is obtained from each of the at least three transmission electron microscope (TEM) observation samples such that a total area of the luminance-obtaining regions is 6.9 μm 2 or more; and
in the step (iv),
the luminance value is relatively corrected by setting a luminance value of the carbon layer to 255 and setting a luminance value of the tungsten layer to 0 to provide the corrected luminance value; and
in the step (v),
for each of the luminance-obtaining regions, an average of absolute value of differences of the corrected luminance values per each pixel is calculated by using a least-square method, and an average of the averaged absolute values is taken as the luminance Sa, or
a luminance Sa is 10 or less, wherein the luminance Sa is calculated by a method comprising the steps of:
(i) preparing transmission electron microscope observation samples of the structure,
(ii) preparing a digital white and black image of a bright-field image of each of the transmission electron microscope observation samples,
(iii) obtaining a luminance value expressed by a numeral value of a tone in color data of each pixel in the digital white and black image,
(iv) correcting the luminance value, and
(v) calculating the luminance Sa by using the corrected luminance value; and
in the step (i),
as the transmission electron microscope observation samples, at least three samples are prepared from the structure,
each of the at least three transmission electron microscope observation samples is prepared by using a focused ion beam method with suppressing a processing damage,
during the focused ion beam method, a carbon layer and a tungsten layer are formed on surface of the structure for prevention of static charge and for sample protection, and
when a direction of the focused ion beam method is taken as a vertical direction, an upper part thickness of each of the samples is 100±30 nm, wherein the upper part thickness of each of the samples is a length of a short axis direction of the surface of the structure in a plane perpendicular to the vertical direction; and
in the step (ii),
the digital white and black image is obtained in each of the at least three transmission electron microscope observation samples,
each of the digital white and black images is obtained by using a transmission electron microscope with a magnification of 100,000 and an acceleration voltage of 200 kV, and includes regions of the structure, the carbon layer, and the tungsten layer,
a luminance-obtaining region is set for each of the digital white and black images, wherein the luminance-obtaining region has a vertical length of 0.5 μm in the vertical direction from the surface of the structure and
each of the digital white and black images is obtained from each of the at least three transmission electron microscope (TEM) observation samples such that a total area of the luminance-obtaining regions is 6.9 μm 2 or more; and
in the step (iv),
the luminance value is relatively corrected by setting a luminance value of the carbon layer to 255 and setting a luminance value of the tungsten layer to 0 to provide the corrected luminance value; and
for the digital white and black image having the luminance value corrected, a noise is removed by using a low-pass filter at a cut-off frequency of 1/(10 pixels); and
in the step (v),
for each of the luminance-obtaining regions, an average of absolute value of differences of the corrected luminance values per each pixel is calculated by using a least-square method, and an average of the averaged absolute values is taken as the luminance Sa.

4. The composite structure according to claim 3 , wherein the luminance Sa is 13 or less when a noise is not removed by using the low-pass filter in step (iv).

5. The composite structure according to claim 1 , wherein an average crystallite size of the polycrystalline ceramic calculated from a tra

Assignees

• Toto Ltd

Inventors

• Iwasawa Junichi
• Ashizawa Hiroaki
• Wada Takuma
• Takizawa Ryoto
• Aoshima Toshihiro
• Takahashi Yuuki
• Kinjo Atsushi

Classifications

• H10P72/0421

  for drying etching · CPC title

• H10P72/7616 Primary

  characterised by a coating, a hardness or a material · CPC title

• H10W74/43

  comprising oxides, nitrides or carbides, e.g. ceramics or glasses · CPC title

• C23C4/04

  characterised by the coating material · CPC title

• C04B2235/96

  Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance · CPC title