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Produce quartz glass and articles thereof

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US5665133A - Process for production of pure transparent quartz - Google Patents

Effective date : Year of fee payment : 4. Year of fee payment : 8. Year of fee payment : It is an object of the present invention to provide a quartz glass jig excellent in the plasma etching resistant characteristics, which does not generate an abnormal etching and particles when used for a plasma generating apparatus. Recently, for the surface treatment of a semiconductor element such as a silicon wafer, etc.

As the plasma etching method, there are a method of introducing a halogen-base corrosive gas such as a fluorine-base, a chlorine-base, etc. On the other hand, introducing a microwave via a microwave-introducing window to form the plasma of the above described halogen-base corrosive gas existing in the chamber, and treating a semiconductor element, a method for introducing a halogen-base corrosive gas and a microwave in a hanging bell-form quartz glass-made bell jar to form the plasma of the halogen-corrosive gas, and treating a semiconductor element for example depositing an insulating thin film on the surface of the semiconductor element is known.

In each treatment, an apparatus of generating plasma is used. Also, for the apparatus, quartz glass jigs are mostly used as a window material for introducing a microwave, a bell jar is used as a plasma-generating chamber and a ring for shielding the apparatus. As a material for these jigs natural quartz glass has been mainly used owing to the good electric characteristics and the high purity.

The surface of the jig, which is brought into contact with plasma, is roughened by mechanical working to stabilize the etching speed and prevent deposits from being released. For above-described roughening a grinding work using a grindstone with ceramic abrasive grains, diamond abrasive grains, silicon dioxide abrasive grains, etc.

The layer or microcrack portion is attacked by radicals formed in the plasma, consequently the microcrack portions only are etched to form abnormally large holes, and in the worst case, there is a fault that the breakage of the quartz glass jig starts from that portions. Also, recently, it has been confirmed that in the above-described plasma, together with the generation of the ions and radicals, abnormally intense ultraviolet rays and electron rays are emitted from the gas, and it has been found that these rays deteriorate the surface of the quartz glass jig, the deteriorated portions becomes the sources of generating particles, and the generated particles deposit on the surface of a semiconductor element to give secondary bad influences.

Furthermore, there is a problem that impurities sometimes enter the microcracks formed by the mechanical working method, and the impurities are volatized at the treatment of a semiconductor element to contaminate the semiconductor element. Also, natural quartz glass sometimes contains many bubbles and thus has the fault that even when the surface is roughened by a chemical method, which does not generate microcracks, the surface thereof is deteriorated by usually intense radiations and electron rays emitted in the plasma, when the bubbles are released and exposed on the surface, the deterioration greatly proceeds at the bubble portions to generate particles, which attach onto the surface of a semiconductor element to deteriorate particularly the dielectric breakdown characteristics.

The object of the invention is to provide a quartz glass jig excellent in the plasma etching resistant characteristics, which gives less abnormal etching and less deterioration of the surface of the quartz glass, and does not give contamination of semiconductor elements by the entrance of impurities.

Also, when the surface roughness Ra is less than 0. When the number of the microcracks of the surface of the jig exceeds the above-described range, the proceed of etching becomes faster by attacking by the radicals generated in the plasma, the microcracks become large, and in the worst case, the breakage of the quartz glass starts from that portion.

The number of the microcracks of the quartz glass surface can be measured by observing the microphotograph. Of course it is even better when no microcrack layer exists on the surface of the quartz glass jig of the invention. In addition to the above-described matters, in the quartz glass of the invention, it is better that the content of bubbles is 0 or 1 as the bubble classification by DIN. When the quartz glass contains bubbles exceeding the above-described range, the bubbles are eroded by the radicals and the ions generated in the plasma and released to become precursors of abnormal holes, and the deterioration further proceeds by the abnormally intense radiations and electron rays in succession thereof to form large holes and generate particles.

The term that the content of bubbles is 0 or 1 as the bubble classification by DIN described above is that according to DIN Deutsche Industrie Norm , the total cross sections cm [] 2 of the bubbles existing in cm 3 are from 0 to 0. Also, when the double refraction amount of the quartz glass exceeds the above-described range, the increase of the density of the quartz glass proceeds by the abnormally intense ultraviolet rays and electron rays irradiated to the twisted portion and microcracks become large.

By establishing the fictive temperature to the above-described range, the density of the quartz glass is lowered to relax the structure, by the irradiation of the abnormally intense ultraviolet rays and electron rays, defects are hard to generate and the increase of the density can be prevented.

In the quartz glass jig of the invention, a fine roughness is formed on the surface as described above, which largely acts on the transmittance of ultraviolet rays. When the transmittance is small, the quartz glass surface is deteriorated by ultraviolet rays. Particularly, The Si-O bond of the quartz glass is broken by abnormally intense ultraviolet rays and electron rays simultaneously generating with the radicals and the ions in the plasma to form a defect, the density becomes high, microcracks become large, the etching speed is greatly accelerated, and large holes are formed.

The above-described inner transmittance means the transmittance, which does not contain the reflection loss at the outer surface of the quartz glass, and the transmittance containing the reflection loss is called an apparent transmittance. As the quartz glass, wherein the bubble classification by DIN is 0 or 1 and the double refraction amount is in the above-described range, there is suitably a synthetic quartz glass obtained by hydrolyzing a silicon compound in the vapor phase.

The measurement of the fictive temperature is by a laser Raman method. The quartz glass jig of the invention is prepared by a natural or synthetic quartz glass as described above, and a synthetic quartz glass, which has less content of bubbles and can be easily obtained as a quartz glass having a high homogeneity, is particularly preferred.

Then, the invention is explained in detail by the practical examples but the examples are shown for illustration and the invention is not limited to those examples.

As shown in FIG. In this case, 10, silicon wafers were treated but an abnormal increase of particles was not confirmed. By carrying out the frost-treatment by the same method as Example 1 except that a natural quartz glass wherein the bubble classification by DIN was 2 was immersed in the frost-treatment liquid used in Example 1, a window material was prepared.

When the etching treatment of Si wafers as in Example 1 was carried out, at the case of treating Si wafers, an abnormal generation of particles was confirmed. The surface of a natural quartz glass wherein the bubble classification by DIN was 2 was subjected to a sand-blast with SiC particles of In the quartz glass obtained, the existence of a microcrack layer was confirmed. A quartz glass window material was prepared using the quartz glass and when the etching treatment of Si wafers was carried out as in Example 1, from the first, particles were generated and the etching treatment could not be carried out.

The synthetic quartz glass was subjected to a hydrogen doping treatment. Then, by applying the frost treatment as in Example 1, a synthetic quartz glass having the surface roughness Ra of 0. When silicon wafers were treated, an abnormal increase of particles was not confirmed. When silicon wafers were treated, an abnormal increase of particles was confirmed. The plasma resistant quartz glass jig described in one of the preceeding claims 1 to 4 , wherein the quartz glass is a synthetic quartz glass obtained by hydrolyzing a silicon compound in the vapor phase.

USB2 en. EPB1 en. KRB1 en. DET2 en. SGA1 en. TWIB en. Optical member made of high-purity and transparent synthetic silica glass and method for production thereof or blank thereof. Moulding having a high content of silicon dioxide, and process for the production of such mouldings.

Cvd jig, manufacture of semiconductor device using the same, and manufacture of the cvd jig. Quartz glass having irregularities on the surface and method for producing the same. Quartz glass member for dry etching and dry etching apparatus equipped with the same. Quartz glass jig having large irregularities on the surface and manufacturing method thereof. EPA2 en. EPA3 en.

DED1 en. KRA en. USA en. CNB en. DET3 en. Method for improving thickness uniformity of deposited ozone-TEOS silicate glass layers.

Enclosure for the treatment, and particularly for the etching of substrates by the reactive plasma method. USB1 en. Methods for protecting silicon or silicon carbide electrode surfaces from morphological modification during plasma etch processing. Apparatus and method for reactive atom plasma processing for material deposition. EPA1 en. Method and apparatus for protection of conductive surfaces in a plasma processing reactor.

CAA en.

Heretofore, a crucible, a jig or the like which is useful for production of a semiconductor single crystal, has been produced by melting a natural quartz powder obtained by pulverizing natural quartz. However, natural quartz contains various metal impurities even when it is of good quality, and, as such, has not been fully satisfactory from the viewpoint of the purity.

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US20020046992A1 - Plasma resistant quartz glass jig - Google Patents

The present invention relates to opaque quartz glass, particularly to opaque quartz glass which is excellent in heat insulation, and adhesiveness to transparent quartz glass. The present invention relates also to a process for producing the quartz glass. Conventionally, opaque quartz glass is produced by heat-fusion of powdery silicate as the source material for vitrification. The process of the heat-fusion includes a Bernoulli process in which the source material is fused in a flame such as an argon-oxygen plasma flame, and oxyhydrogen flame; and a vacuum fusion process in which silica packed in a container is heated and fused under a high vacuum. The opaque quartz glass is produced conventionally from natural silica rock or low-quality quartz as the source material.

Preparation and Existing States of La/Al Co-Doped Quartz Powders

The present invention relates to transparent quartz glass of high purity produced by molding powdery amorphous silica, and sintering and fusing the molded article of amorphous silica. Particularly, the present invention relates to pure transparent quartz glass which contains less impurities like alkalis respectively at a content of not more than 1 ppm, contains less water, and has high heat resistance, thereby being useful for a photomask and other uses in semiconductor production. Conventionally, transparent quartz glass is produced by a process of melting powdery quartz crystal in vacuo in a furnace, a process of melting powdery quartz crystal by oxyhydrogen flame, or a like process. However, the conventional processes employ powdered natural quartz crystal, whereby the resulting quartz glass is not satisfactory to meet the severe requirements for high purity for highly integrated LSI, even though the quartz glass has high heat resistance. Although the powdered natural quartz crystal is treated for high purity, not all of the undesired impurities can be removed to respective contents of not higher than 1 ppm at the moment. To obtain higher purity of the quartz glass, processes are investigated, including a VAD process which sinters deposited synthetic amorphous silica, and a sol-gel process which sinters powdery amorphous silica obtained by hydrolysis of a silicic acid alkoxide. However, the synthetic powdery amorphous silica, although it can be produced in higher purity, gives quartz glass inferior in heat resistance to the one obtained from natural quartz material, disadvantageously.

SEE VIDEO BY TOPIC: Q2 What makes glass different from a solid such as quartz?
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Customs Tariff Number Chapter 70 - Search results (172)

Method for producing a quartz glass crucible having a roughened inner surface region for pulling single crystal silicon. Patent number: Abstract: The present invention is a method for producing a quartz glass crucible for pulling a single crystal silicon from a silicon melt held therein, including the steps of: producing a quartz glass crucible having an outer layer including an opaque quartz glass containing bubbles therein and an inner layer including a transparent quartz glass containing substantially no bubbles; roughening a region of an inner surface of the produced quartz glass crucible, the region being in contact with the silicon melt when holding the silicon melt; and heating the quartz glass crucible having the roughened inner surface to crystallize a surface of the roughened region.

EFFECT: technological advantages, low temperature coefficient of linear expansion and high heat resistance, stability of dielectric characteristics in a wide range of temperatures, and moisture when attainment of high strength characteristics. SUBSTANCE: non-calcinated quartz ceramics is obtained by preparation of slip from broken quartz glass, formation of raw workpiece by method of casting into gypsum forms, impregnation of raw workpiece with water solution and drying impregnated workpiece. EFFECT: simplification of non-calcination technology of quartz ceramics and increase of ceramics strength.

By the combination of a three-axis system to move the glass sample and a fast 3D system to move the laser focus, the SLE process is now suitable to produce more complex structures in a shorter time. Here we present investigations which enabled the new possibilities. We started with investigations of the optimum laser parameters to enable high selective laser-induced etching: surprisingly, not the shortest pulse duration is best suited for the SLE process. Secondly we investigated the scaling of the writing velocity: a faster writing speed results in higher selectivity and thus higher precision of the resulting structures, so the SLE process is now even suitable for the mass production of 3D structures. Finally we programmed a printer driver for commercial CAD software enabling the automated production of complex 3D glass parts as new examples for lab-on-a-chip applications such as nested nozzles, connectors and a cell-sorting structure. Pure transparent materials such as quartz glass fused silica glass can be processed to generate 3D structures in a subtractive 3D printing process similar to 3D lithography using the glass as positive-tone resist [ 1 ]. The exposure is executed by scanning focused ultrashort pulsed fs or ps laser radiation inside the glass changing its properties locally in the focal volume. The development is executed by subsequent wet-chemical etching an acid such as HF or an alkaline such as KOH or similar materials in water. Depending on the processing conditions, the etching rate of the laser-modified material can be much larger than the untreated glass, e. The fundamentals of the process, some applications and also its combination with other ultrafast 3D writing technologies can be found in reviews such as [ 2 , 3 , 4 ] and the references therein. The state of the art is that 3D microchannels and complex movable 3D precision parts can be produced in quartz silica glass and that the SLE process is possible in plenty of transparent materials, both in crystals such as sapphire, quartz, YAG and in glasses such as borosilicate glass e.

A synthetic quartz powder obtained by calcining a powder of silica gel, for use in a high temperature region of at least ° C. and for the production thereof. As a method for producing a synthetic quartz glass powder to satisfy the present Ltd. Synthetic silica glass articles and a method for manufacturing them.

Method of producing quartz ceramics and articles thereof

The invention relates to methods for producing high-density ceramic materials based on quartz glass - quartz ceramics with open porosity close to zero. Such material will find wide application for products operating in difficult thermal and climatic conditions. Currently, methods for producing quartz ceramics and articles from it for the manufacture of steel pouring glasses and dispensers in metallurgy are well known R. Churakova, E. Fedorova, Yu. Polonsky, E. Ermolaeva, A. Pivinsky, E. Suzdaltsev, Quartz ceramics and refractories, , vol.

US805303A - Producing hollow quartz-glass articles. - Google Patents

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WO2000024685A1 - Synthetic quartz glass and method for production thereof - Google Patents

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Glass Articles, of which the following is a specificatioxi'. For producing hollow glass articles the glass-blower usually 'takes on an iron tube ID the 'pipe alum of "melted glass out of the glass-pot in the ace and turns the wipe. Quartzglass req'uirestofbe heated u 1 tea rature exceeding 2, centigra e bef0!

Customs Tariff Number Chapter 70 - Search results Cullet and other waste and scrap of glass; glass in the mass excl.

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