CN201006856Y - Freely formed silex glass ingot - Google Patents
Freely formed silex glass ingot Download PDFInfo
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- CN201006856Y CN201006856Y CNU2006200032592U CN200620003259U CN201006856Y CN 201006856 Y CN201006856 Y CN 201006856Y CN U2006200032592 U CNU2006200032592 U CN U2006200032592U CN 200620003259 U CN200620003259 U CN 200620003259U CN 201006856 Y CN201006856 Y CN 201006856Y
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Abstract
The utility model discloses a quartz glass product in the form of blank, ingot or plate, the total defect concentration of the utility model is lower than 150 defects/cm<3> and hydroxyl group concentration is lower than 150ppm. The quartz glass product is formed by firing super pure silica which is used as raw material, wherein the quartz glass blank, ingot or plate is freely formed on a platen rotating around the same axis as the raw material quartz product.
Description
The cross reference of related application
This application requires the right of priority of the US 60/689507 of submission on June 10th, 2005, and this patent application is incorporated herein by reference fully at this.
Technical field
The present invention relates to the silica glass ingot with low impurity content and fabricating low-defect-density of use in semiconductor machining is used.This silica glass ingot is made as raw material by the quartz ware that uses direct drawing.
Background technology
Be used for that the semiconductor wafer course of processing that microchip makes need comprise order and the multiple step, as mask, deposition and etching.In etching step, wafer and the etched chamber of generation are exposed in the erosion environment condition, as active-ion-etch and plasma etching.Because the erosion performance of etch process, thereby, in order to carry out reliable wafer process, must the careful material of selecting etching chamber.Thereby the most inboard etching chamber parts are normally made by silica glass.In theory, the pure silica glass of etching only can go out to discharge silicon and oxygen.Than transition metal and other elements can change wafer composition and thereby change the semiconductor property of wafer, silicon and oxygen are less to the harm of wafer.
An example of chamber part is a quartz window.In a kind of structure, quartz window is as the dividing plate between the chamber atmosphere and the energy.Because this window is arranged at the top of wanting etched semiconductor wafer usually, should be chemical pure as much as possible so require quartz window, promptly contain the impurity that is lower than 50ppm.Also require this window to have low-down bulk defects density, these bulk defectss for example are tramp material inclusion and bubble.When this bulk defects is exposed in the etching atmosphere of quartz window surface, can causes uneven etching, thereby produce silica glass particle this window.Free particulate matter in the etching chamber can cause serious harm to wafer.With respect to the etch features on the wafer surface (about 50 nanometers), this particulate size (1～10 micron) makes this particle have sizable potential destructiveness.These particles can stop up the grid (gate) on the wafer and destroy conductive channel on the wafer, and wafer is polluted by impurity element.Thereby the chip etching chamber needs can be slowly and etching and can not produce the particulate quartz window equably.
Use known in the state of the art is made quartzy ingot based on the flame melt method of sand (sand-based).Usually, this method relate to supply with the quartzy material of particulate state by or near the oxygen fuel flame, thereby form block glass ingot gradually by process of growth with relative low deposition rate, this sedimentation rate for example is 5 Pounds Per Hours or lower.Under whole energy that the advantage of flame melt method is to make individual particle be exposed to thermal source.Yet, the shortcoming of this orientated deposition method be to make each particle to be exposed in the feeder system and furnace atmosphere in dirt, each sand grains all might form defective in ingot.Single sand grains is exposed under the influence of product (water) of thermal radiation and combustion reactions of oxygen fuel flame.This influence has produced the quartz ware of hydroxyl concentration greater than 150ppm, and this has changed melten glass and viscosity temperature correlation, thereby has limited its end-use.
Disclosed application JP-61122131A discloses the glass ingot of a kind of glass ingot manufacturing installation and manufacturing thereof.U.S. Patent No. 4612023 discloses a kind of method of making no striped, no bubble and uniform quartz glass plate.U.S. Patent No. 6415630 discloses a kind of evenly equipment of quartz glass plate without stripes of making, and wherein crucible and quartz glass bar relatively move perpendicular to the longitudinal axis of rod.
In the prior art, quartz glass bar can be used as raw material to form bigger glass shape.Yet, still can exist with material and pile up and overlapping relevant boundary defect.In a kind of existing method, used a kind of cascade type structure (the soften glass layer is successively stacked up) to come build-up materials, this method can cause boundary defect because of multiple reason.These defectives comprise the bubble of folded band, the discrete impurity particle of being carried secretly, the impurity atom of being carried secretly and fold line.Need extra process to reduce or remove this defective in this melts.In addition, this operation need use fireproof die or container to form the net shape of glass ingot.The refractory materials that contacts with the melten glass ingot is the dirt sources that can cause defective in this ingot.In addition, the mismatch of thermal expansion can cause slabbing or crack between fused silica glass and the refractory materials in this ingot.
Still need the ultra low defect quartz ware that can be used for making the parts in the semiconductor processing, promptly hydroxyl concentration is lower than 150ppm and overall defect density (diameter greater than 10 microns bubble and inclusion) and is lower than 150/cm
3Ingot.
Summary of the invention
The present invention relates to a kind of by firing the method that forms the silica glass ingot of ultra low defect and impurity as the high-purity quartz goods of raw material, wherein silica glass ingot with the platen of the coaxial rotation of raw material quartz ware on freely form.
In one embodiment, the present invention relates to a kind ofly form overall defect density and be lower than 50 defective/cm by firing high-purity quartz goods as raw material
3And hydroxyl concentration is lower than the method for the silica glass ingot of 50ppm, wherein silica glass ingot with the platen of the coaxial rotation of raw material quartz ware on freely form.
The invention further relates to overall defect density and be lower than 50 defective/cm
3And hydroxyl concentration is lower than the quartz glass product of forms such as the ingot, plate, base of 50ppm.
Description of drawings
Fig. 1 is the synoptic diagram of embodiment that is used to make the device of quartz glass product of the present invention.
Embodiment
When with herein the time, represent that proximate word can be used for modifying any can change and the quantitaes that can not cause relative basic function to change.Therefore, use the numerical value of modifying such as the term of " approximately " and " basically " can be not limited to specified in some cases accurate numerical value.
When with herein the time, quartz glass product is meant can process or make the various size of quartzy bases such as annular, flange shape, tabular, plate-like, window-like and quartz glass plate, ingot and the base etc. of thickness with it.
When using herein, " silica glass ingot " is meant the finished product of the present invention, and it can be that overall defect density is lower than 50/cm
3And hydroxyl concentration is lower than the forms such as base, ingot and plate of 50ppm.Quartzy ingot of the present invention can be used for the window component of semiconductor machining chamber.
When with herein the time, term " refluxes (reflow) " and is meant that the material that is similar to quartz or glass softens at it and becomes the intrinsic procedure of can be in the effect current downflow/fusion of himself weight and being carried out when again himself being distributed.
When with herein the time, defective is meant diameter greater than 10 microns bubble or inclusion, and overall defect density is meant the overall number of defective in the unit volume.Defective can detect by the random site up-sampling (for example being sliced form) from quartzy ingot, and can with the naked eye check under magnifying glass.Defective is counted, and overall defect number and the population of samples by a plurality of samples amasss calculating overall defect density then.
Make the raw material of quartzy ingot:
When using herein, raw material of quartz glass is meant any Prefabricated stone quartz glass article, and it can be forms such as rod, pipe, and it has solid or tubular cross-section, and the numbers of sides of its shape of cross section can from 3 limits in the scope on infinite many limits, but also comprise circular cross sectional shape.In one embodiment, the cross section of raw material of quartz glass is solid and is circle.In another embodiment, raw material of quartz glass is the quartz glass bar that directly draws.
When using herein, " quartz glass bar " is meant any Prefabricated stone quartz glass article that is used as raw material in the present invention, and it can be that cross section is solid or tubular rod and pipe etc.In one embodiment, the shape of cross section as the Prefabricated stone quartz glass article of raw material has at least 3 limits.In another embodiment, this ready-formed raw material of quartz glass is the bar with circular solids in cross-section.In one embodiment, the diameter of this glass stick at 1mm between the 100mm.In another embodiment, the external diameter of this glass stick at 20mm between the 50mm.
In one embodiment, make this quartz glass bar by natural quartz crystal as raw material.In another embodiment, make this rod by synthetic silicon.In the 3rd embodiment, this raw material comprises natural quartz crystal rod and the rod that is made by synthetic silicon.In one embodiment, this raw material of quartz glass is SiO
2Content is the Prefabricated stone quartz glass article of 85wt% at least.In another embodiment, this prefabricated glasswork is solid or the piped elongated shape, and it forms by soot body (soot body) or by any other high purity particulate matter sintering that flame hydrolysis makes.
After the raw materials melt step, can further anneal to remove hydroxyl (OH) base and OH base concentration is reduced to about 50ppm to the controlled length of quartz glass bar.The surface and/or the end pre-treatment of cleaning step have been considered rod section (rod segment) is comprised.The known connection that can realize glass stick in this area by conical end regions.In one embodiment of the invention, the end of the bar-shaped raw material section of silica glass forms required end shape, carries out pre-washing then before pre-connection and semicontinuous ingot fusion step.This pre-wash step any one in can be in several ways finished, and these modes include but not limited to that pickling, washing composition clean or its any combination.
Make the method for quartzy ingot:
With reference now to the synoptic diagram of Fig. 1,, it has been described the fusion among the present invention or has fired equipment.The raw material of this method is represented with the form of quartz pushrod 10.The end of the quartzy ingot of finally making 11 is supported on the platen 7, makes its longitudinal axis be positioned on the vertical position.In one embodiment, platen 7 is positioned at (not shown) on the horizontal revolving stage.Platen 7 utilizes drive shaft 8 to rotate around vertical axis, and this drive shaft 8 is connected on the suitable speed-changing driving device (not shown) with any known configuration, for example is connected on the motor.In one embodiment, for further this bar raw material 10 of local heating of energy, be provided with fireproof shelves hot plate and furnace roof (not shown).
In one embodiment, the vertical axis of the longitudinal axis of raw material 10 and platen 7 (with selectable turntable) is concentric, makes their axis substantial registration, for example aims at coaxially.Thereby the longitudinal axis of the ingot of finally making 11 is aimed at similarly with the axis of raw material 10 and platen 7, so that carry out axisymmetric reflux course.In another embodiment, the maximum eccentricity between the axis of raw material and ingot is not more than one times raw material diameter.
Setting fires/and heating source 5 to be to be implemented in 1400 ℃ to 2400 ℃ silica glass work/softening/yield temperatures in the scope.Heating source 5 can be following any or its combination: resistive heating, radio frequency heating, induction heating, microwave heating, LASER HEATING, electron beam heating, zone heating, plasma torch heating or burner.
As in the embodiment illustrated in fig. 1, use burner 5 to reflux bigger ingot that heat is provided as bar-like raw material 10.Light this burner, and by flame column with the heat transferred refractory furnace.In one embodiment, burner is " oxy-fuel burner (oxy-fuelburner) ", to its supply such as inflammable gas of hydrogen, carbon monoxide, methane or propane with such as the combustion-supporting gas of air or oxygen.Burner can be for this purpose and a normally used class burner that for example part has the burner that multitube is constructed in the central.In addition, this burner can have surface mixing, partly-premixed closing or comprehensive premixed structure.
In one embodiment, the design of burner and structure are as disclosed in the U.S. Patent No. 5934893 that is entitled as " Burner andUtilization of Such Burner in Glass Furnace (burner and in the application in the glass-melting furnace) ".In another embodiment, heating source 5 moves time enough with respect to bar-like raw material 10, thoroughly to fire raw material 10.Can change translational speed along with the process of firing, thereby keep the optimum size stability of product ingot.In an embodiment again, heating source 5 comprises a plurality of burner (not shown), as single center of top burner, a plurality of sidepiece burner and a plurality of tops side burner, wherein fire for the best of optimizing bar-like raw material, sidepiece burner and top side burner is spaced apart.
Furnace atmosphere can comprise air or inertia or rare gas.The smelting furnace shell can heat by radiation or induction.In one embodiment, before bar-like raw material being inserted, preheat by 5 pairs of refractory furnace 6 of burner for backflow.In one embodiment, at first wash the inside of smelting furnace with rare gas element.In next step, monolithic bar-like raw material 10 is added in the top of reflow furnaces, arrive downwards on the platen pedestal 7 of rotation then, bar-like raw material 10 forms bigger ingot 11 on this platen pedestal 7.Along with 10 fusions of every rod become bigger ingot 11, add extra fuel rod, keep the rotational symmetry of rod and fusion ingot simultaneously.The interpolation speed of fuel rod depends on the temperature of this process and the formation speed of fusion ingot 11.
In one embodiment, realize continuous feeding in the following way: with the bar partial melting, take out not fused length, insert new fuel rod then.In another embodiment, realize continuous feeding by the bar-shaped feed that molten prepolymer connects, so that carry out the melting process of semicontinuous ingot.In an embodiment again, in a kind of successive process, be bigger ingot by the direct fusion of bar-like raw material.When this rod by continuously elongated and when directly joining in of the present invention method as raw material 10 it, by in smelting furnace, under the temperature of fusion between 1800 ℃ and 2500 ℃, keeping coming fused quartz sand in about 1 to 10 hour, thereby make this bar-like raw material.
In one embodiment, with fuel rod of different nature (for example fuel rod that makes by natural silicon) with by synthesizing the fuel rod alternate feed that silicon makes, so that produce the quartzy ingot of the laminate structure of alternating layer with more low-quality quartz material and higher quality quartz material.In the embodiment of coat structure, the higher quality material of the inside of this ingot is made by the raw material of higher quality, and its outside is made by more inferior raw material.
Along with more silica glass material is piled up, bigger fusion ingot 11 stow away from heats 5 move down with certain speed, and its translational speed makes the outside diameter of this ingot be freely formed with a kind of controllable manner.In case formed acceptable big ingot 11, then bar-like raw material 10 stops charging, thereby and the end face of ingot flatten because of the heat supply of burner continues to flow.At last, stop the heat supply of thermal source 5, from smelting furnace, take out ingot 11 then, and cooling is so that carry out aftertreatment and inspection.
In one embodiment, silica glass ingot 11 is with per hour 5 to 50 pounds speed fusing.In another embodiment, silica glass ingot is with every little 10 to 20 pounds speed fusing.
In rotational symmetry reflux course of the present invention, because the outside surface of rod becomes the outside surface of fused the finished product, so the possibility of backflow defective is extremely low in the fusion ingot.Fused the finished product main body avoids the impurity that may carry defective secretly and/or may exist in feeder system or furnace atmosphere.Because the rotational symmetry method has stoped the stacked in succession or layering of raw material, so it is extremely low to form interfacial possibility in the finished product of ingot.
In addition, " be freely formed " in the method for ingot, do not need container or mould to form or keep the diameter and/or the shape of ingot in the present invention.Help to reduce the possibility of refractory materials pollutent in the ingot without mould (making by the refractory brick material usually), also reduced indirect material cost simultaneously.In addition, the ingot that is freely formed of the present invention unlikely breaks because of the stress relevant with thermal expansion mismatch between silica glass ingot and the fireproof die material.Though do not need the ingot mould tool, platen 7 comprises raised brim, and this raised brim is arranged so that this edge does not have molded or is shaped this finished product ingot.
In the housekeeping operation of back, to remove the end sections that directly contacts with fire-resistant platen 7 in the finished product ingot 11 usually.
Ingot by method making of the present invention:
As mentioned above, use direct tensile quartz glass bar in the method for the invention, rather than use the fused quartz particle in the orientated deposition process, the rank that the fusion quality among the present invention remains on height and effectively controls as raw material.Because bar-like raw material is directly drawn in smelting furnace, and before it is drawn into the fusion goods, the quartz sand raw material melts under the temperature of fusion between 1800 ℃ to 2500 ℃ and keeps about 1 to 10 hour residing permanently the time of staying, therefore the chemical property of the silica glass bar that is drawn is very even, and the density of the bulk defects as inclusion or bubble is very low.
The overall defect density of the quartz glass product of forms such as the ingot of the bar-like raw material manufacturing that the use defect concentration is low, plate, base is lower than every cubic centimetre of 150 defectives and hydroxyl concentration is lower than 150ppm.In another embodiment, every cubic centimetre of prepared glass ingot is lower than 50 defectives and hydroxyl concentration is lower than 50ppm.In another embodiment, every cubic centimetre on this ingot is lower than 150 defectives and hydroxyl concentration is lower than 50ppm.In the 4th embodiment, every cubic centimetre is lower than 50 defectives and hydroxyl concentration is lower than 150ppm.
In one embodiment, the hydroxyl concentration of prepared glass ingot is lower than 30ppm, is higher than the hydroxyl concentration of quartz raw material.In one embodiment, the hydroxyl concentration of ingot is lower than 20ppm, is higher than the hydroxyl concentration as the quartz pushrod of raw material.
Except very high fusion quality and favourable economically fusion speed, method of the present invention can also the large-sized quartz glass product of fusion.In one embodiment, these goods are the glass ingot form of cylindrical shape, and its external diameter is between 6 inches to 24 inches, and height is between 6 inches to 24 inches.In the 3rd embodiment, the diameter of formed silica glass ingot is 2 to 100 times as the diameter of the quartz glass bar of raw material.In another embodiment, the diameter of ingot is 5 to 50 times of diameter of bar-like raw material.In another embodiment, its diameter is 5 to 20 times of diameter of bar-like raw material.
Embodiment: the invention will be further described by following non-restrictive example:
Embodiment 1: the quartzy ingot that the use that will buy (or also can buy from St.Gobain) from Tosoh makes based on the flame melt method of sand is as comparative example.
Embodiment 2: use method of the present invention, to make diameter be 12 inches to " 214 type " quartz pushrod that will buy from General Electric Company and highly be 10 inches ingot as raw material.214 type quartz pushrods are characterised in that the temperature profile of high purity, improvement and low thermal expansivity, and (OH) content is lower than 20ppm.
From quartzy ingot, cut the section that diameter is 3 " and thickness is about 1/4 " at random, measure OH concentration and defect level then.Using infrared beamsplitter to carry out OH measures.Under magnifying glass, with the naked eye measure overall defect density.The results are shown in the following table.
| Embodiment | OH(ppm) | Overall defect density (#/cm 3) |
| 1. based on the flame melt method of sand | 150～200 | ＞150 |
| 2 rotational symmetry free formings | ＜50 | ＜50 |
This printed instructions utilizes embodiment to come open the present invention, comprises best mode, but also makes any technician in this area can both make and use the present invention.The scope of patentability of the present invention is determined by claim, and can be comprised other embodiment that can expect for those skilled in the art.If these other embodiment have the structural element identical with the character express of claim, do not have the different equivalent construction element of essence if perhaps they comprise with the character express of claim, mean that so these embodiment also should comprise within the scope of the claims.All cited literature 2s of reference herein all clearly are hereby incorporated by.
Claims (3)
1. the quartz glass product of a base, ingot or plate form, its overall defect density is lower than 150 defective/cm
3And hydroxyl concentration is lower than 150ppm.
2. according to the quartz glass product of claim 1, its overall defect density is lower than 50 defective/cm
3And hydroxyl concentration is lower than 50ppm.
3. the quartz glass product of an ingot forms has intermediate core and outside, and this outside external diameter is between 6～24 inches, and wherein, the diameter of this intermediate core is at least 1/2 of this external diameter, and its overall defect density is lower than 150 defective/cm
3And hydroxyl concentration is lower than 150ppm.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US68950705P | 2005-06-10 | 2005-06-10 | |
| US60/689507 | 2005-06-10 | ||
| US11/266638 | 2005-11-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN201006856Y true CN201006856Y (en) | 2008-01-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNU2006200032592U Expired - Lifetime CN201006856Y (en) | 2005-06-10 | 2006-03-16 | Freely formed silex glass ingot |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN201006856Y (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105841757A (en) * | 2016-05-04 | 2016-08-10 | 合肥江航飞机装备有限公司 | Method for controlling nozzle diameter of glass nozzle flowmeter |
-
2006
- 2006-03-16 CN CNU2006200032592U patent/CN201006856Y/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105841757A (en) * | 2016-05-04 | 2016-08-10 | 合肥江航飞机装备有限公司 | Method for controlling nozzle diameter of glass nozzle flowmeter |
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