CN104986967A - Fused quartz surface treatment device and method - Google Patents
Fused quartz surface treatment device and method Download PDFInfo
- Publication number
- CN104986967A CN104986967A CN201510275557.0A CN201510275557A CN104986967A CN 104986967 A CN104986967 A CN 104986967A CN 201510275557 A CN201510275557 A CN 201510275557A CN 104986967 A CN104986967 A CN 104986967A
- Authority
- CN
- China
- Prior art keywords
- fused quartz
- pending
- protective film
- sample table
- plasma
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Sampling And Sample Adjustment (AREA)
- Surface Treatment Of Glass (AREA)
Abstract
The invention provides a fused quartz surface treatment device and method. The fused quartz surface treatment device includes a reaction chamber equipped shell. The top center of the shell is equipped with a plasma generation unit. The bottom center of the shell is provided with a sample platform. The center position of the sample platform is provided with an isolation unit, which comprises a protective film and an isolation cover. The protective film is spread between the sample platform and to-be-treated fused quartz. The isolation cover is placed around the to-be-treated fused quartz on the protective film. The fused quartz surface treatment device provided by the invention can isolate the to-be-treated fused quartz from the surrounding to avoid metal sputtering pollution from the device shell and the sample platform. Meanwhile, through two plasma etching, the subsurface damage layer of the fused quartz can be removed so as to obtain fused silica with good surface roughness.
Description
Technical field
The present invention relates to optical material processing technique field, more particularly, relate to a kind of fused quartz surface-treated device and method.
Background technology
Fused quartz applies the most general optical material in large-scale high power laser system, and fused quartz material is widely used in preparing the optical elements such as lens, window and shield blade in optical system.In the fused quartz optical material course of processing, need to carry out grinding and polishing, and for the grinding of traditional fused quartz optical substrate and polishing processing, because abrasive material to exist the effect of mechanical force to fused quartz substrate surface, can at the sub-surface damage of the sub-surface layer Formation Depth of fused quartz substrate in micron dimension.Along with fused quartz is in the widespread use in the fields such as light laser, space optics, X-ray optics, in the urgent need to there is no sub-surface damage and ganoid fused quartz substrate.
At present, after grinding and polishing processing, the technology of removal fused quartz substrate sub-surface damage commonly used comprises: based on the wet etching of hydrofluoric acid, MRF and ion beam polishing.Wherein, hf etching technology, by the chemical action of hydrofluoric acid and fused quartz, can remove the defect layer on surface fast; But because hf etching is isotropic, sub-surface damage such as crackle and cut etc. can be expanded along with the carrying out of etching, thus cause surface irregularity.MRF utilizes magnetic polishing liquid under the influence of a magnetic field, and form flexible polishing film, flexible polishing film only has tangential force to fused quartz surface, does not almost have normal force, so can not produce sub-surface damage; But, hydrolysis layer can be formed on fused quartz surface after MRF, and residual a large amount of magnetic polishing particle, these residual MRF contaminating impurities also can cause damage from laser under laser irradiation.Based on the defect that above-mentioned two kinds of processing technologies exist, ion beam polishing technology, owing to introducing sub-surface damage, becomes the main method obtaining ganoid fused quartz substrate; But, because it is very low to the etch rate of fused quartz, therefore, the sub-surface damage that ion beam polishing technology removes fused quartz should not be used alone.
In recent years, the work utilizing inductively coupled plasma (Inductively Coupled Plasma, hereinafter referred to as ICP) reactive ion etching technology to remove fused quartz sub-surface damage layer aspect increases gradually.Chemical reaction combines with physical bombardment by reactive ion etching technology, makes etching have good directivity and etch rate faster.The usual using plasma reaction unit of reactive ion etching technology realizes, this device top passes into gas and produces plasma body, sample to be etched is placed in the bottom corresponding with top, and be top electrode with top, bottom sample platform is lower electrode, under upper/lower electrode electric field action, make plasma bombardment sample surfaces to be etched, complete etching process.But, carry out in surface-treated process utilizing reactive ion etching technology to fused quartz, the particle of fused quartz surface attachment and the foreign matter such as metal sputtering pollution from etching system vacuum cavity, can react with reactant gases, catalysis forms the polymer deposition being difficult to etch, cause the roughen of etching sample surfaces, form the radiation injury of induced by plasma at sample surfaces.
At present, in order to the radiation injury in inhibited reaction ion etching, most of technology is all angularly optimized the reactive ion etching characteristic of fused quartz from the plenum system of reactive ion etching gas standard (kind and proportioning), etching working vacuum degree, working gas.Although metallic pollution can be suppressed to a certain extent, but, all can not fundamentally solve metal sputtering pollution problem, thus fused quartz surface formation radiation injury in reactive ion etching cannot be solved, namely solve the problem of fused quartz surface roughen in reactive ion etching.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of fused quartz surface-treated device and method, with realize remove fused quartz sub-surface damage layer while, avoid surface formed radiation injury, obtain the fused quartz of better surfaceness.
The invention provides a kind of fused quartz surface-treated device, comprising:
There is the housing of reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
Preferably, the material of described inner walls is aluminium, anodised aluminium or stainless steel.
Preferably, described plasma generation unit comprises:
Be arranged on the gas storage cavity of described case top central position;
The vent line be connected with described gas storage cavity;
Be centered around the radio-frequency coil around described gas storage cavity.
Preferably, the material of described sample table is aluminium or anodised aluminium.
Preferably, described protective film is polyimide film; The thickness of described protective film is 50 μm ~ 60 μm.
Preferably, described cage is fused quartz glass cover; The thickness of described cage is 2mm ~ 6mm.
Present invention also offers a kind of fused quartz surface-treated method, comprise the following steps:
Pending fused quartz is placed in fused quartz surface-treated device, through twice plasma etching, obtains the fused quartz after surface treatment;
Described fused quartz surface-treated device comprises: the housing with reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
Preferably, described first time the gas of plasma etching be 50sccmAr, operating pressure is 0.1Pa ~ 0.3Pa, and plasma power is 750W ~ 800W, and accelerating power is 120W ~ 180W, and self-deflection voltage is 200V ~ 230V, and the time is 8min ~ 15min.
Preferably, the gas of described second time plasma etching is (25sccm ~ 45sccm) Ar/ (5sccm ~ 25sccm) CHF
3, operating pressure is 0.1Pa ~ 0.3Pa, and plasma power is 700W ~ 1100W, and accelerating power is 120W ~ 180W, and self-deflection voltage is 240V ~ 290V, and the time is 8min ~ 15min.
Preferably, the described Cheng Qian be excessively placed on by pending fused quartz in fused quartz surface-treated device, also comprises:
Pending fused quartz is carried out surface cleaning.
The invention provides a kind of fused quartz surface-treated device and method, described fused quartz surface-treated device comprises: the housing with reaction chamber; Described case top central position is provided with plasma body generating unit; Described housing bottom central position is provided with sample table; Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.Compared with prior art, pending fused quartz is first placed in isolated location by fused quartz surface-treated device provided by the invention, pending fused quartz and surrounding sample table are isolated with the housing with reaction chamber, and the pending surface of described pending fused quartz is corresponding with the plasma generation unit that described case top central position is arranged; The plasma body produced by plasma generation unit again, through twice plasma etching, obtains the fused quartz after surface treatment.Pending fused quartz and surrounding can be isolated by fused quartz surface-treated device provided by the invention, avoid the metal sputtering from device case and sample table to pollute, reduce the radiation injury in reactive ion etching; Meanwhile, by twice plasma etching, first can remove foreign matters such as the particles of pending fused quartz surface attachment, then remove the sub-surface damage layer of fused quartz, obtain the fused quartz of better surfaceness.Experimental result shows, adopts fused quartz surface-treated device and method provided by the invention, and after carrying out the sub-surface damage layer removal of fused quartz, the fused quartz surfaceness obtained is 0.2nm.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only embodiments of the invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to the accompanying drawing provided.
The structural representation of the fused quartz surface-treated device that Fig. 1 provides for the embodiment of the present invention;
The structural representation of the fused quartz surface-treated device that Fig. 2 provides for the embodiment of the present invention 1;
The vertical view of the fused quartz surface-treated device cage that Fig. 3 provides for the embodiment of the present invention 1;
Fig. 4 is the fused quartz surface atom power Photomicrograph after surface treatment that the embodiment of the present invention 1 obtains;
The XPS spectrum figure on the surface of the fused quartz after surface treatment that Fig. 5 is fused quartz pending in the embodiment of the present invention 2, obtain in embodiment 2 and the fused quartz after surface treatment that comparative example obtains;
Fig. 6 is the stereoscan photograph on the surface of the fused quartz after surface treatment that the fused quartz after surface treatment that obtains in the embodiment of the present invention 2 and comparative example obtain;
Fig. 7 is the optical microscope photograph after fused quartz after the surface treatment that obtains of the embodiment of the present invention 1 ~ 3 amplifies defect.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described technical scheme of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
The invention provides a kind of fused quartz surface-treated device, comprising:
There is the housing of reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
Refer to Fig. 1, the structural representation of the fused quartz surface-treated device that Fig. 1 provides for the embodiment of the present invention, wherein, 1 is housing, 2 is plasma body generating unit, and 3 is sample table, and 4 is isolated location, 5 is pending fused quartz, and 6 is protective film, and 7 is cage.
In the present invention, described housing (1) has reaction chamber, for carrying out plasma etching; In the present invention, the material of described housing (1) inwall is preferably aluminium, anodised aluminium or stainless steel, is more preferably anodised aluminium.
In the present invention, described housing (1) top center is provided with plasma body generating unit (2), for generation of plasma body.In the present invention, described plasma generation unit (2) preferably includes: the gas storage cavity being arranged on described housing (1) top center; The vent line be connected with described gas storage cavity; Be centered around the radio-frequency coil around described gas storage cavity.In the present invention, described gas storage cavity is arranged on described housing (1) top center, directly communicates with described housing (1); Described vent line is connected with described gas storage cavity, the gas for generation of plasma body can be passed into gas storage cavity; Described radio-frequency coil is centered around around described gas storage cavity, for generation of plasma body.
In the present invention, described housing (1) bottom centre position is provided with sample table (3), described sample table (3) is corresponding with the plasma body generating unit (2) being arranged on housing (1) top center, and described sample table (3) is lower electrode, the plasma body generating unit (2) corresponding with described sample table (3) is top electrode; Under electric field action, the plasma body produced in the gas storage cavity of plasma body generating unit (2) is made to realize accelerating.In the present invention, the material of described sample table (3) is preferably aluminium or anodised aluminium, is more preferably anodised aluminium.
In the present invention, described sample table (3) central position is provided with isolated location (4), for the pending fused quartz (5) be placed in isolated location and surrounding being isolated.In the present invention, described isolated location (4) is arranged on described sample table (3) central position, object is that pending fused quartz (5) is placed between sample table (3) lower electrode and plasma body generating unit (2) top electrode correspondence position, is convenient to carry out plasma etching to pending fused quartz (5).
In the present invention, described isolated location (4) comprises protective film (6) and cage (7); Described protective film (6) is laid between described sample table (3) and pending fused quartz (5); Described cage (7) is placed on the upper pending fused quartz (5) of protective film (6) around.In the present invention, described protective film (6) is laid between described sample table (3) and pending fused quartz (5), and the tiled area of protective film (6) is greater than pending fused quartz (5) put area, object makes protective film (6) can after placement cage (7), pending fused quartz (5) bottom surface and side are isolated with sample table (3) and housing (1), only that the pending surface of pending fused quartz (5) is corresponding with the plasma generation unit (2) that described housing (1) top center is arranged.In the present invention, protective film is preferably polyimide film; The source of the present invention to described protective film is not particularly limited, and adopts the commercial goods of above-mentioned polyimide film well known to those skilled in the art.In the present invention, the thickness of described protective film is preferably 50 μm ~ 60 μm, is more preferably 55 μm.
In the present invention, described cage (7) is placed on the upper pending fused quartz (5) of protective film (6) around; Described cage (7) is not for having the tubular structure of end face and bottom surface, and the size of the present invention to described end face and bottom surface is not particularly limited.In the present invention, described cage (7) is placed on protective film (6), bottom surface is covered by protective film (6) completely, end face is not closed, form semi-enclosed isolated location (4), make the pending fused quartz (5) be placed in described isolated location (4), can be corresponding with described plasma generation unit (2), thus carry out plasma etching.In the present invention, described cage (7) is preferably fused quartz glass cover; The thickness of described cage is preferably 2mm ~ 6mm, is more preferably 5mm.
The fused quartz surface-treated device provided according to the invention described above embodiment, can remove the sub-surface damage layer of fused quartz; Meanwhile, avoid surface to form radiation injury, obtain the fused quartz of better surfaceness.Embodiment of the present invention working process is as follows:
First pending fused quartz (5) is placed in the isolated location (4) of sample table (3) central position, protective film (6) and the sample table (3) of described pending fused quartz (5) underrun isolated location (4) are isolated, described pending fused quartz (5) side is isolated with housing (1) by the cage (7) of isolated location (4), and the pending surface of described pending fused quartz (5) is corresponding with the plasma generation unit (2) that described housing (1) top center is arranged; Carry out plasma etching again, the plasma body produced by plasma generation unit (2) is under electric field acceleration effect, plasma etching is carried out to the pending surface of described pending fused quartz (5), obtains fused quartz after surface treatment.
Present invention also offers a kind of fused quartz surface-treated method, comprise the following steps:
Adopt fused quartz surface-treated device, pending fused quartz is placed in fused quartz surface-treated device, through twice plasma etching, obtains the fused quartz after surface treatment;
Described fused quartz surface-treated device comprises: the housing with reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
In the present invention, identical with described in technique scheme of described fused quartz surface-treated device, does not repeat them here.The present invention is not particularly limited described pending fused quartz, adopts after well known to those skilled in the art, grinding and polished finish with the fused quartz glass of sub-surface damage.
In the present invention, the described Cheng Qian be excessively placed on by pending fused quartz in fused quartz surface-treated device, preferably also comprises:
Pending fused quartz is carried out surface cleaning.In the present invention, the process of described surface cleaning preferably specifically comprises the following steps:
By pending fused quartz successively through dipping, flushing and oven dry, obtain the fused quartz through surface cleaning.In the present invention, first flooded in scavenging solution by pending fused quartz, object removes the impurity of pending fused quartz surface attachment; The time of described dipping is preferably 25min ~ 35min, is more preferably 30min.The method of the present invention to described dipping is not particularly limited, the technical scheme adopting ultrasonic immersing well known to those skilled in the art or directly soak.In the present invention, described scavenging solution is preferably acetone or volume ratio is the vitriol oil of 2:1 and the mixing solutions of hydrogen peroxide, is more preferably acetone.
After completing described dipping, the fused quartz after dip treating rinses by the present invention, and object removes scavenging solution residual on fused quartz.In the present invention, the washing fluid that described flushing is used is preferably deionized water; The temperature of described flushing is preferably 70 DEG C ~ 90 DEG C, is more preferably 80 DEG C; The time of described flushing is preferably 4min ~ 6min, is more preferably 5min.
After completing described flushing, the present invention is dried through the fused quartz rinsed after process, obtains the fused quartz through surface cleaning.The method of the present invention to described oven dry is not particularly limited, and adopts baking oven well known to those skilled in the art to toast.In the present invention, the temperature of described oven dry is preferably 100 DEG C ~ 120 DEG C, is more preferably 110 DEG C; The time of described oven dry is preferably 25min ~ 35min, is more preferably 30min.
In the present invention, pending fused quartz is placed in fused quartz surface-treated device, through twice plasma etching, obtains the fused quartz after surface treatment.Plasma etching of the present invention and reactive ion etching, adopt fused quartz surface-treated device provided by the invention, first pending fused quartz is placed in the isolated location of sample table central position, then in the plasma body generating unit of case top central position, gas is passed into, generate plasma body, under electric field acceleration effect, plasma body carries out physical bombardment to pending fused quartz, complete first time plasma etching, gas is passed into again in plasma body generating unit, generate plasma body, under electric field acceleration effect, plasma carries out second time plasma etching to pending fused quartz, complete the surface treatment of fused quartz.
In the present invention, described first time plasma etching object be removed the foreign matter such as dust, water of fused quartz remained on surface by physical bombardment.In the present invention, described first time plasma etching gas be preferably 50sccmAr; Described first time, the operating pressure of plasma etching was preferably 0.1Pa ~ 0.3Pa, was more preferably 0.2Pa; Described first time, the plasma power of plasma etching was preferably 750W ~ 800W, was more preferably 780W; Described first time, the accelerating power of plasma etching was preferably 120W ~ 180W, was more preferably 150W; Described first time, the self-deflection voltage of plasma etching was preferably 200V ~ 230V, was more preferably 220V; The time of plasma etching described first time is preferably 8min ~ 15min, is more preferably 10min.
In the present invention, the object of described second time plasma etching removes the sub-surface damage layer of fused quartz.In the present invention, the gas of described second time plasma etching is preferably (25sccm ~ 45sccm) Ar/ (5sccm ~ 25sccm) CHF
3, be more preferably 45sccmAr/5sccmCHF
3; The operating pressure of described second time plasma etching is preferably 0.1Pa ~ 0.3Pa, is more preferably 0.2Pa; The plasma power of described second time plasma etching is preferably 700W ~ 1100W, is more preferably 800W ~ 1000W; The accelerating power of described second time plasma etching is preferably 120W ~ 180W, is more preferably 150W; The self-deflection voltage of described second time plasma etching is preferably 240V ~ 290V, is more preferably 250V; The time of described second time plasma etching is preferably 8min ~ 15min, is more preferably 10min.
The invention provides a kind of fused quartz surface-treated device and method, described fused quartz surface-treated device comprises: the housing with reaction chamber; Described case top central position is provided with plasma body generating unit; Described housing bottom central position is provided with sample table; Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.Compared with prior art, pending fused quartz is first placed in isolated location by fused quartz surface-treated device provided by the invention, pending fused quartz and surrounding sample table are isolated with the housing with reaction chamber, and the pending surface of described pending fused quartz is corresponding with the plasma generation unit that described case top central position is arranged; The plasma body produced by plasma generation unit again, through twice plasma etching, obtains the fused quartz after surface treatment.Pending fused quartz and surrounding can be isolated by fused quartz surface-treated device provided by the invention, avoid the metal sputtering from device case and sample table to pollute, reduce the radiation injury in reactive ion etching; Meanwhile, by twice plasma etching, first can remove foreign matters such as the particles of pending fused quartz surface attachment, then remove the sub-surface damage layer of fused quartz, obtain the fused quartz of better surfaceness.Experimental result shows, adopts fused quartz surface-treated device and method provided by the invention, and after carrying out the sub-surface damage layer removal of fused quartz, the fused quartz surfaceness obtained is 0.2nm.
In order to further illustrate the present invention, be described in detail below by following examples.Following examples of the present invention fused quartz used is JGS1 type fused quartz glass.
Embodiment 1
The structural representation of the fused quartz surface-treated device that embodiment 1 provides as shown in Figure 2.Wherein, 1 is housing, and 2 is plasma body generating unit, and 3 is sample table, and 4 is isolated location, and 5 is pending fused quartz, and 6 is protective film, and 7 is cage, and 8 is gas storage cavity, and 9 is vent line, and 10 is radio-frequency coil.
Described housing (1) has reaction chamber, and the material of inwall is aluminium.Described housing (1) top center is provided with plasma body generating unit (2), and described plasma generation unit (2) comprises gas storage cavity (8), vent line (9) and radio-frequency coil (10).Described gas storage cavity (8) is arranged on housing (1) top center, directly communicate with described housing (1), described vent line (9) is connected with described gas storage cavity (8), and described radio-frequency coil (10) is centered around around described gas storage cavity.Described housing (1) bottom centre position is provided with sample table (3), and material is anodised aluminium, and described sample table (3) is corresponding with plasma body generating unit (2).Described sample table (3) central position is provided with isolated location (4), and described isolated location (4) comprises protective film (6) and cage (7).Described protective film (6) is the polyimide film of 55 μm for thickness, is laid between described sample table (3) and pending fused quartz (5); Described cage (7) for thickness be the fused quartz glass cover of 5mm, be placed on the upper pending fused quartz (5) of protective film (6) around, described cage (7) is not for having the tubular structure of end face and bottom surface, as shown in Figure 3, the vertical view of fused quartz surface-treated device cage that provides for the embodiment of the present invention 1 of Fig. 3.
The fused quartz surface-treated device adopting above-described embodiment 1 to provide carries out the surface treatment of fused quartz, and concrete steps are:
(1) by pending fused quartz acetone ultrasonic immersion 30min, then use the deionized water rinsing 5min of 80 DEG C, then put into 110 DEG C of baking oven baking 30min, obtain the fused quartz through surface cleaning.
(2) the above-mentioned fused quartz through surface cleaning is placed in the isolated location (4) of fused quartz surface-treated device sample table (3) central position that embodiment 1 provides, then by vent line (9), 50sccmAr is passed in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 780W, generate plasma body, then be 150W at electric field acceleration power, self-deflection voltage is under 220V effect, plasma body carries out physical bombardment 10min to fused quartz, complete first time plasma etching.
(3) vent line (9) is continued through by 45sccmAr/5sccmCHF
3pass in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 1000W, generate plasma body, then electric field acceleration power be 150W, under self-deflection voltage is 250V effect, plasma body carries out physical bombardment 10min to fused quartz, completes second time plasma etching, obtain the fused quartz after surface treatment, remove the sub-surface damage layer 9 μm of fused quartz.
Adopt the surfaceness of DI Innova type atomic force microscope to the fused quartz after surface treatment that embodiment 1 obtains to detect, detected result as shown in Figure 4.Fig. 4 is the fused quartz surface atom power Photomicrograph after surface treatment that the embodiment of the present invention 1 obtains, and as shown in Figure 4, the surfaceness of the fused quartz after surface treatment that the embodiment of the present invention 1 obtains is 0.2nm.
Embodiment 2
The fused quartz surface-treated device adopting above-described embodiment 1 to provide carries out the surface treatment of fused quartz, and concrete steps are:
(1) be that the vitriol oil of 2:1 and the mixing solutions of hydrogen peroxide soak 30min by pending fused quartz volume ratio, then use the deionized water rinsing 5min of 80 DEG C, then put into 110 DEG C of baking oven baking 30min, obtain the fused quartz through surface cleaning.
(2) the above-mentioned fused quartz through surface cleaning is placed in the isolated location (4) of fused quartz surface-treated device sample table (3) central position that embodiment 1 provides, then by vent line (9), 50sccmAr is passed in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 780W, generate plasma body, then be 150W at electric field acceleration power, self-deflection voltage is under 220V effect, plasma body carries out physical bombardment 10min to fused quartz, complete first time plasma etching.
(3) vent line (9) is continued through by 25sccmAr/25sccmCHF
3pass in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 800W, generate plasma body, then electric field acceleration power be 150W, under self-deflection voltage is 250V effect, plasma body carries out physical bombardment 10min to fused quartz, completes second time plasma etching, obtain the fused quartz after surface treatment, remove the sub-surface damage layer 3.92 μm of fused quartz.
Detect the surfaceness of fused quartz, detected result shows, the surfaceness 0.2nm of the fused quartz after surface treatment that the embodiment of the present invention 2 obtains.
Embodiment 3
The fused quartz surface-treated device adopting above-described embodiment 1 to provide carries out the surface treatment of fused quartz, and concrete steps are:
(1) by pending fused quartz acetone ultrasonic immersion 30min, then use the deionized water rinsing 5min of 80 DEG C, then put into 110 DEG C of baking oven baking 30min, obtain the fused quartz through surface cleaning.
(2) the above-mentioned fused quartz through surface cleaning is placed in the isolated location (4) of fused quartz surface-treated device sample table (3) central position that embodiment 1 provides, then by vent line (9), 50sccmAr is passed in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 780W, generate plasma body, then be 150W at electric field acceleration power, self-deflection voltage is under 220V effect, plasma body carries out physical bombardment 10min to fused quartz, complete first time plasma etching.
(3) vent line (9) is continued through by 35sccmAr/15sccmCHF
3pass in gas storage cavity (8), maintenance operating pressure is 0.2Pa, the plasma power arranging radio-frequency coil (10) is again 800W, generate plasma body, then electric field acceleration power be 150W, under self-deflection voltage is 250V effect, plasma body carries out physical bombardment 10min to fused quartz, completes second time plasma etching, obtain the fused quartz after surface treatment, remove the sub-surface damage layer 3.72 μm of fused quartz.
Detect the surfaceness of fused quartz, detected result shows, the surfaceness 0.2nm of the fused quartz after surface treatment that the embodiment of the present invention 3 obtains.
Comparative example
Isolated location (4) in fused quartz surface-treated device embodiment 1 provided removes, and with this device, surface treatment is carried out to fused quartz, concrete steps, with reference to embodiment 2, obtain the fused quartz after surface treatment, remove the sub-surface damage layer 3.92 μm of fused quartz.
Adopt the surface of ESCALAB 250 model x-ray photoelectron spectroscopy to the fused quartz after surface treatment that the fused quartz after surface treatment obtained in fused quartz pending in the embodiment of the present invention 2, embodiment 2 and comparative example obtain to carry out XPS detection, detected result as shown in Figure 5.The XPS spectrum figure on the surface of the fused quartz after surface treatment that Fig. 5 is fused quartz pending in the embodiment of the present invention 2, obtain in embodiment 2 and the fused quartz after surface treatment that comparative example obtains, wherein, fused quartz pending in (a) embodiment 2, the b fused quartz after surface treatment that () comparative example obtains, the fused quartz after surface treatment obtained in (c) embodiment 2.As shown in Figure 5, the fused quartz surface-treated device that the embodiment of the present invention 2 provides effectively can avoid metallic pollution, thus makes the surface treated fused quartz obtained have good surfaceness.
The surface of FEI Sirion200 type scanning electronic microscope to the fused quartz after surface treatment that the fused quartz after surface treatment obtained in the embodiment of the present invention 2 and comparative example obtain is adopted to carry out scanning electron microscope analysis, as shown in Figure 6.Fig. 6 is the stereoscan photograph on the surface of the fused quartz after surface treatment that the fused quartz after surface treatment that obtains in the embodiment of the present invention 2 and comparative example obtain, wherein, the a fused quartz after surface treatment that () comparative example obtains, the fused quartz after surface treatment obtained in (b) embodiment 2.As shown in Figure 6, the fused quartz surface-treated device that the embodiment of the present invention 2 provides, by suppressing metallic pollution, has increased substantially the fused quartz surface quality after surface treatment, and the fused quartz surface emissivity damage after the surface treatment obtained is few, keeps smooth.
For the difference of the fused quartz after the surface treatment that further comparing embodiment 1 ~ 3 obtains, fused quartz after the surface treatment obtain embodiment 1 ~ 3 proceeds surface etch with the hydrofluoric acid that concentration is 40% respectively, to be amplified in the defect that fused quartz surface occurs, then Nikon OPTIPHOT-100 type opticmicroscope is adopted to observe, as described in Figure 7.Fig. 7 is the optical microscope photograph after fused quartz after the surface treatment that obtains of the embodiment of the present invention 1 ~ 3 amplifies defect, wherein, fused quartz after a surface treatment that () obtains for embodiment 2, fused quartz after b surface treatment that () obtains for embodiment 3, the fused quartz after the surface treatment that (c) obtains for embodiment 1.As shown in Figure 7, carrying out in plasma etching, the smooth degree on the fused quartz surface after the content effects on surface process of Ar gas has impact, is namely optimized helpful to not destroying fused quartz smooth surface degree while of removal fused quartz sub-surface damage to a certain extent to gas mixing ratio.
The above-mentioned explanation of the disclosed embodiments, enables professional and technical personnel in the field realize or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a fused quartz surface-treated device, is characterized in that, comprising:
There is the housing of reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
2. device according to claim 1, is characterized in that, the material of described inner walls is aluminium, anodised aluminium or stainless steel.
3. device according to claim 1, is characterized in that, described plasma generation unit comprises:
Be arranged on the gas storage cavity of described case top central position;
The vent line be connected with described gas storage cavity;
Be centered around the radio-frequency coil around described gas storage cavity.
4. device according to claim 1, is characterized in that, the material of described sample table is aluminium or anodised aluminium.
5. device according to claim 1, is characterized in that, described protective film is polyimide film; The thickness of described protective film is 50 μm ~ 60 μm.
6. device according to claim 1, is characterized in that, described cage is fused quartz glass cover; The thickness of described cage is 2mm ~ 6mm.
7. a fused quartz surface-treated method, is characterized in that, comprises the following steps:
Pending fused quartz is placed in fused quartz surface-treated device, through twice plasma etching, obtains the fused quartz after surface treatment;
Described fused quartz surface-treated device comprises: the housing with reaction chamber;
Described case top central position is provided with plasma body generating unit;
Described housing bottom central position is provided with sample table;
Described sample table central position is provided with isolated location, and described isolated location comprises protective film and cage; Described protective film is laid between described sample table and pending fused quartz; Described cage to be placed on protective film around pending fused quartz.
8. the method according to right 7, it is characterized in that, described first time, the gas of plasma etching was 50sccmAr, operating pressure is 0.1Pa ~ 0.3Pa, plasma power is 750W ~ 800W, accelerating power is 120W ~ 180W, and self-deflection voltage is 200V ~ 230V, and the time is 8min ~ 15min.
9. the method according to right 7, is characterized in that, the gas of described second time plasma etching is (25sccm ~ 45sccm) Ar/ (5sccm ~ 25sccm) CHF
3, operating pressure is 0.1Pa ~ 0.3Pa, and plasma power is 700W ~ 1100W, and accelerating power is 120W ~ 180W, and self-deflection voltage is 240V ~ 290V, and the time is 8min ~ 15min.
10. the method according to any one of claim 7 ~ 9, is characterized in that, the described Cheng Qian be excessively placed on by pending fused quartz in fused quartz surface-treated device, also comprises:
Pending fused quartz is carried out surface cleaning.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510275557.0A CN104986967B (en) | 2015-05-26 | 2015-05-26 | A kind of device and method of fused quartz surface treatment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510275557.0A CN104986967B (en) | 2015-05-26 | 2015-05-26 | A kind of device and method of fused quartz surface treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104986967A true CN104986967A (en) | 2015-10-21 |
| CN104986967B CN104986967B (en) | 2017-07-25 |
Family
ID=54298892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510275557.0A Active CN104986967B (en) | 2015-05-26 | 2015-05-26 | A kind of device and method of fused quartz surface treatment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104986967B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277814A (en) * | 2016-07-28 | 2017-01-04 | 中国工程物理研究院激光聚变研究中心 | A kind of processing method on fused quartz optical component surface |
| CN114149180A (en) * | 2021-12-07 | 2022-03-08 | 中国科学院上海光学精密机械研究所 | Processing method for improving damage threshold of fused quartz component |
-
2015
- 2015-05-26 CN CN201510275557.0A patent/CN104986967B/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277814A (en) * | 2016-07-28 | 2017-01-04 | 中国工程物理研究院激光聚变研究中心 | A kind of processing method on fused quartz optical component surface |
| CN106277814B (en) * | 2016-07-28 | 2019-04-05 | 中国工程物理研究院激光聚变研究中心 | A kind of processing method on fused quartz optical component surface |
| CN114149180A (en) * | 2021-12-07 | 2022-03-08 | 中国科学院上海光学精密机械研究所 | Processing method for improving damage threshold of fused quartz component |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104986967B (en) | 2017-07-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7736998B2 (en) | Silicon-on insulator substrate and method for manufacturing the same | |
| TWI575594B (en) | Method of cleaning aluminum plasma chamber parts | |
| JP4225908B2 (en) | Reactive atomic plasma processing method for material deposition | |
| KR101332206B1 (en) | Semiconductor processing | |
| US20090258159A1 (en) | Novel treatment for mask surface chemical reduction | |
| CN107721196A (en) | Method for removing surface chemical structure defects of fused quartz component | |
| CN104986967A (en) | Fused quartz surface treatment device and method | |
| CN106277814B (en) | A kind of processing method on fused quartz optical component surface | |
| KR20210038952A (en) | Glass composite, casing, display device and terminal device | |
| JP2005303255A (en) | Low-reflectance processing method of silicon substrate for solar cells | |
| JP6275206B2 (en) | Improved quality multispectral zinc sulfide | |
| JP2010034156A (en) | Texture forming method and vacuum processing equipment | |
| CN112071740B (en) | Method for preparing silicon carbide structure by picosecond laser irradiation | |
| JPH07180091A (en) | Aluminum sheet, its production and deposition preventive cover using the sheet | |
| Lens et al. | Mechanism of the immobilization of surfactants on polymer surfaces by means of an argon plasma treatment: influence of UV radiation | |
| CN113578858B (en) | Cleaning device and cleaning method | |
| CN103871865B (en) | A kind of method of cleaning plasma reaction chamber sidewall | |
| KR20110102197A (en) | Method for removing residues on surfaces of float glass | |
| Pakpum et al. | Redeposition-free of silicon etching by CF4 microwave plasma in a medium vacuum process regime | |
| JP2007036170A (en) | Low-reflectance processing method of silicon substrate for solar cells and silicon substrate for solar cell | |
| JP4890668B2 (en) | Quartz glass lid for reaction apparatus for semiconductor heat treatment and manufacturing method thereof | |
| CN116462419A (en) | Surface treatment process for improving laser damage threshold of fused quartz element | |
| WO2007049347A1 (en) | Low reflectivity machining method for solar cell silicon substrate, and solar cell silicon substrate | |
| Zhang et al. | Study on Damage Characteristics of Fused Silica under Ion Beam Sputtering and AMP Technique | |
| CN116444167A (en) | Etching method for improving ultraviolet laser induced damage resistance of fused quartz element |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20201211 Address after: 230000 building 3, No.1, Kechuang Town, Changlinhe Town, Feidong County, Hefei City, Anhui Province Patentee after: Anhui Zhongke Grating Technology Co.,Ltd. Address before: 230026 Jinzhai Road, Baohe District, Hefei, Anhui Province, No. 96 Patentee before: University of Science and Technology of China |