CN109661379A - Form the laser system and method with the high purity fused silica glass piece of micro- sawtooth - Google Patents
Form the laser system and method with the high purity fused silica glass piece of micro- sawtooth Download PDFInfo
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- CN109661379A CN109661379A CN201780050627.XA CN201780050627A CN109661379A CN 109661379 A CN109661379 A CN 109661379A CN 201780050627 A CN201780050627 A CN 201780050627A CN 109661379 A CN109661379 A CN 109661379A
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- recess
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1453—Thermal after-treatment of the shaped article, e.g. dehydrating, consolidating, sintering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K26/00—Working by laser beam, e.g. welding, cutting or boring
- B23K26/352—Working by laser beam, e.g. welding, cutting or boring for surface treatment
- B23K26/3568—Modifying rugosity
- B23K26/3584—Increasing rugosity, e.g. roughening
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
- C03C23/0025—Other surface treatment of glass not in the form of fibres or filaments by irradiation by a laser beam
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C4/00—Compositions for glass with special properties
- C03C4/0092—Compositions for glass with special properties for glass with improved high visible transmittance, e.g. extra-clear glass
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K2103/00—Materials to be soldered, welded or cut
- B23K2103/50—Inorganic material, e.g. metals, not provided for in B23K2103/02 – B23K2103/26
- B23K2103/54—Glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1484—Means for supporting, rotating or translating the article being formed
- C03B19/1492—Deposition substrates, e.g. targets
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/02—Pure silica glass, e.g. pure fused quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/20—Doped silica-based glasses containing non-metals other than boron or halide
- C03C2201/23—Doped silica-based glasses containing non-metals other than boron or halide containing hydroxyl groups
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/06—Doped silica-based glasses
- C03C2201/30—Doped silica-based glasses containing metals
- C03C2201/34—Doped silica-based glasses containing metals containing rare earth metals
- C03C2201/3488—Ytterbium
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2201/00—Glass compositions
- C03C2201/80—Glass compositions containing bubbles or microbubbles, e.g. opaque quartz glass
Abstract
A kind of sintering is included in the step of high purity fused silica soot on piece rasterizes laser beam with a thickness of 500 μm or the system and method for smaller thin high purity fused silica glass piece;Wherein, the pattern of rasterisation includes the target position of the tight spacing on sheet material, when being observed on cross section, laser is sintered soot and forms small recess in the first main surface of sheet material simultaneously, wherein the small recess is zigzag, so that at least some recesses have the top surface of generally platform with generally flat bottom surface and at least some corresponding adjacent crowns, the top surface is deviateed by the side wall at steep angle with bottom surface.
Description
Cross reference to related applications
This application claims the U.S. Provisional Application Ser submitted the 62/376,701st priority power on the 18th of August in 2016
Benefit is included in herein based on content of the application and by its full text herein, is illustrated as complete below.
Background technique
The present disclosure relates generally to the formation containing silica article, and in particular to the formation of thin silicon dioxide sheet glass.Two
Silica soot can be generated by the method for such as flame hydrolysis etc.Silica soot is then sinterable transparent to be formed
Or partially transparent sheet glass.
Summary of the invention
Some embodiments of the disclosure are related to high purity fused silica glass piece comprising the first main surface and
Second main surface opposite with first main surface.The sheet glass is at least the silica of 99.9 moles of %, wherein titanium dioxide
Silicon is at least generally amorphous, thus has the crystalline content less than 1 weight %.Between first main surface and the second main surface
Average sheet thickness less than 500 μm.First main surface has the small recess along the first main surface in cross-section, wherein respectively
The depth of small recess be at least 25nm and be no more than 1 μm, the depth relative on the either side of respective notches it is adjacent part hat
The higher person measurement in shape object, each small recess have the width for being at least 5 μm between adjacent local crown, and each small
The length of recess is at least 500 μm.
In some embodiments, the recess is zigzag, so that at least some recesses have generally flat bottom
Surface and at least some corresponding adjacent crowns have the top surface of generally platform, and the top surface of the generally platform is logical
The side wall and bottom surface for crossing into steep angle deviate.
In some embodiments, along the first main surface, at least 10 small recesses are respectively other at least one
Small recess difference is within 1000 μm.
In some embodiments, at least three recesses are arranged in a row side by side each other, the depth of each recess with this three
Within the mean depth difference 20% of recess.
In some embodiments, the small recess is along its curved in length.In some such embodiments, small recessed
The curve and straight line of mouth deflect at least 10 degree.In some such embodiments, curve is along the length of small recess at 500 μm
Distance in turn at least 10 degree but no more than 360 degree.In some embodiments, each small recess at steering position is turning to
Place maintains separately from each other.In some embodiments, the direction bending that each small recess is continuously turned to along the length of small recess
At least 90 degree.In some embodiments, curve is usually formed the polygon with sphering vertex.
In some embodiments, width of each recess between each local crown is at least 50 μm, wherein described
The small respective depth of recess is at least 100nm but is no more than 500nm, and the depth is relative to the phase on the either side of respective notches
The higher person measurement in adjacent local crown.In some such embodiments, the length of each recess is at least 2500 μm.
The other embodiments of the disclosure are related to the electronic device comprising thin substrate, and the thin substrate includes with a thickness of 500 μ
M or smaller high purity fused silica piece.The high purity fused silica piece has recess in its main surface,
Described in recess be zigzag so that at least some recesses have the bottom surface of general planar and at least some corresponding adjacent hats
Shape object has the top surface of substantially platform, and the top surface of the substantially platform passes through the side wall and bottom surface at steep angle
Deviate.The electronic device further includes metal layer, and recess is connect and covered with thin substrate, wherein the metal layer towards sawtooth
Downside is textured into a certain pattern, the geometry inverse correlation of the pattern and sawtooth, so that high purity fused silica piece
Main surface on crown correspond to metal layer downside on recess, and the recess on the downside of metal layer correspond to substrate
High purity fused silica piece main surface on crown.
In some embodiments, the recess is small recess, and the depth of each recess is at least 25nm and is no more than 1 μ
M, the depth is relative to the higher person measurement in the adjacent local crown on the either side of respective notches, wherein each recess exists
There is the width for being at least 5 μm, and the length of each recess is at least 500 μm between adjacent local crown.
In some embodiments, metal layer directly contacts thin substrate.In some such embodiments, metal layer is straight
Contact the high purity fused silica piece of thin substrate.
In some embodiments, Bao Jicai with a thickness of 200 μm or smaller.
In some embodiments, the porosity of high purity fused silica piece is less than 10 volume %.
The other embodiments of the disclosure are related to a kind of sintering with a thickness of 500 μm or smaller thin high-purity consolidation dioxy
The method of SiClx sheet glass.The method includes rasterizing laser beam in the on piece of high purity fused silica soot
(raster) the step of.The pattern of rasterisation includes the target position of the tight spacing on sheet material, when being observed on section,
Laser is sintered soot and forms recess in the first main surface of sheet material simultaneously, wherein the recess is zigzag, makes
Bottom surface of at least some recesses with general planar and at least some corresponding adjacent crowns are obtained with substantially platform
The top surface of top surface, the substantially platform is deviateed by the side wall at steep angle with bottom surface.In some such realities
It applies in mode, wherein the recess is small recess, the depth of each recess is at least 25nm and is no more than 1 μm, the depth phase
For the higher person measurement in the adjacent local crown on the either side of respective notches, wherein each recess is in adjacent part hat
There is the width for being at least 5 μm, and the length of each recess is at least 500 μm between shape object.
In some embodiments, the pattern includes to be generally the mobile laser beam of the shape of polygon, wherein polygon
The vertex of shape shape is sphering.
Other feature and advantage are given in the following detailed description, Partial Feature and advantage therein are to this field
It will be appreciated that for technical staff, or by implementing printed instructions and its claims and attached reality described in figure
It applies mode and is realized.
It should be understood that foregoing general description and following description are all only exemplary, and it is intended to
Offer understands the property of claims and the overview of feature or frame.
Appended attached drawing, which provides, to be further understood, and attached drawing is incorporated in the present specification and constitutes part of specification.
Attached drawing instantiates one or more embodiments, and is used to explain the principle and operation of each embodiment together with specification.
Detailed description of the invention
Fig. 1 shows the laser sintering system according to an illustrative embodiments.
Fig. 2 shows the laser sintering systems according to another illustrative embodiments.
Fig. 3 shows the laser sintering system according to another illustrative embodiments.
Fig. 4 shows the laser sintering system according to another illustrative embodiments.
Fig. 5 is shown according to an illustrative embodiments to the laser sintered titanium dioxide by laser sintered formation
The output situation of Zhai Ke (Zygo) optical profilometer that the surface of silica glass piece measures.
Fig. 6 is shown according to another illustrative embodiments to the laser sintered dioxy by laser sintered formation
The output situation for the Zhai Ke optical profilometer that the surface of SiClx sheet glass measures.
Fig. 7 is the laser sintered silica glass piece table by laser sintered formation an of illustrative embodiments
The 3D minute yardstick schematic diagram for measuring profile in face.
Fig. 8 A-8C is the atomic force microscopy that the glass sheet surface of Fig. 7 is shown according to an illustrative embodiments
Mirror profile scan situation.
Fig. 9 shows the Zhai Keguang that the surface of the earth silicon material after surface polishing to non-laser sintering measures
The comparison for learning contourgraph exports situation.
Figure 10, which is shown, is formed by laser burning by various laser sintering processes according to illustrative embodiments
The amplification surface image on the silica glass piece surface of knot.
Figure 11 is the three-dimensional surface profile obtained from the vertical perspective of the sheet glass of an illustrative embodiments.
Figure 12 is the figure of the two dimensional surface profile obtained from the three-dimensional surface profile of Figure 11.
Figure 13 is the three-dimensional surface profile of the Figure 11 obtained from perspective view.
Figure 14 is the concept map of micro- sawtooth according to an illustrative embodiments.
Figure 15 is the three-dimensional surface profile obtained from the vertical perspective of the sheet glass of another illustrative embodiments.
Figure 16 is the figure of the two dimensional surface profile obtained from the three-dimensional surface profile of Figure 15.
Figure 17 is the three-dimensional surface profile of the Figure 15 obtained from perspective view.
Figure 18 is the three-dimensional surface profile obtained from the vertical perspective of the sheet glass of another illustrative embodiments.
Figure 19 is the figure of the two dimensional surface profile obtained from the three-dimensional surface profile of Figure 18.
Figure 20 is the three-dimensional surface profile of the Figure 18 obtained from perspective view.
Figure 21 is the concept map of the electronic device according to an illustrative embodiments.
Specific embodiment
Attached drawing is generally referred to, silica glass piece/material through oversintering and related system and side are shown
Each embodiment of method.In each embodiment, system and method disclosed herein utilize one or more glass soots
Generating means (such as flame hydrolysis burner), be intended to or be intended to for glass soot particles stream to be transmitted to soot deposit device or
To form glass soot piece on soot deposit surface.Then using laser sintered soot piece to form silica glass piece.One
As for, laser beam is directed to soot on piece so that soot densify, to form dioxy that is fully sintered or partially sintering
SiClx sheet glass.In each embodiment, to glass soot generating means, soot deposit surface and/or the structure for being sintered laser
It makes and/or operates and configured, with the silica glass compared to some sintering formed by the silica soot being sintered
Piece (such as compared to furnace technology or torch technique and some other laser sintering process), being formed has very high surface smooth
The sheet glass of the sintering of degree.In some embodiments, sheet glass forming method discussed herein is formed by silica glass
The surface characteristics of glass piece differ markedly from by polishing silica surface (such as by polishing silica ingot
(boule) surface) surface characteristics.
In addition, to glass soot generating means, soot deposit surface and/or the construction and/or the operation progress that are sintered laser
Configuration, it is described to form the sheet glass of the sintering of certain pollutants (such as sodium (Na), surface hydroxyl etc.) with extremely low level
Pollutant is typically found in be formed by earth silicon material using some other methods.It has been found that in some implementations
In mode, by using laser sintering processes discussed herein and system, the silica glass piece of sintering can have high table
Face smoothness and low pollutant load are without additional polishing step.
With reference to Fig. 1, which shows the dioxy for being used to form high-purity, high glossy according to an illustrative embodiments
The system and method for SiClx sheet glass.As shown in Figure 1, system 10 includes soot deposit device, shown with depositing drum 12, this is heavy
Product drum 12 has external sediment surface 14.System 10 include soot generating means, with soot burner 16 (such as flame hydrolysis combustion
Burner) it shows, glass soot particles stream 18 is directed on deposition surface 14 to form glass soot piece 20.
As shown in Figure 1, drum 12 rotates in a clockwise direction, so that soot piece 20 is advanced with the machine direction that arrow 22 indicates
It leaves drum 12 and advances through sintering laser 24.In some embodiments, soot piece 20 is in the direction of arrow 22
Tensional state (such as axial tension).In a particular embodiment, soot piece 20 is only in the direction of arrow 22 in stretching
State (such as axial tension), not apply tension in the transverse direction of soot piece 20.Applicant have surprisingly discovered that during sintering
It does not need to make to burn soot piece cross directional stretch to keep surface characteristics discussed herein (specially roughness).However, at least some
In other embodiments, soot piece 20 is in stretching in a lateral direction.In some embodiments, different directions are selected
On stretching to control the bending or warpage of the soot piece of sintering.
As will be explained in greater, sintering laser 24 generates the laser beam 26 towards soot piece 20, and comes from
Glass soot piece is sintered into the sheet glass 28 being partially or fully sintered by the energy of laser beam 26.As should be understood, from sintering
The sheet glass 28 that the energy of laser beam 26 causes the fine and close chemical conversion of glass soot piece 20 to be partially or fully sintered.Specifically, titanium dioxide
Soot particles are heated rapidly to the temperature higher than soot fusing point using laser 24 by the laser sintered of silicon soot piece 20, due to molten
The reflux for melting soot particles has formd fully dense thin silica glass piece 28.
In each embodiment, the initial density of soot piece 20 in 0.2g/cc between 0.8g/cc, and titanium dioxide
Silica glass piece 28 is the fully sintered silica glass piece that density is about 2.2g/cc (such as 2.2g/cc increase and decrease 1%).Such as
It is explained in greater detail below, in some embodiments, silica glass piece 28 is the complete burning comprising hole or bubble
The silica glass piece of knot, therefore the density of the sheet material is less than 2.2g/cc.In each other embodiments, soot piece 20
Initial density in 0.2g/cc between 0.8g/cc, and silica glass piece 28 is density in 0.2g/cc to 2.2g/cc
Between the silica glass piece partially sintered.
In each embodiment, the length and width of the sheet glass 28 of sintering in 1mm between 10m, specific real
It applies in mode, at least one of length and width of sheet glass 28 of sintering is greater than 18 inches.In each embodiment, recognize
Allow to be formed by the length of the sheet glass 28 of sintering for system 10 and/or width dimensions are greater than formed by other methods two
The full-size of silica structure (such as silica ingot, full-size are usually limited to less than 18 inches).
System 10 is configured to create the soot piece 20 with smooth surface topology, and being converted to equally has smooth table
The sheet glass 28 of face topological.In each embodiment, soot burner 16 be positioned in from drum 12 it is sizable with a distance from simultaneously
And/or person and drum 12 are angled, so that soot stream 18 forms the soot piece 20 with smooth upper surface.This positioning method
It is re-depositing on surface 14 so that soot stream 18 first mixes.In a particular embodiment, the outlet nozzle of soot burner 16
14 1 inches from deposition surface to 12 inches, particularly 1 inch to 4 inches are located in, more particularly about 2.25 inches of position
Place, and/or positioned relative to soot deposit surface 14 at 30-45 degree angle.It in a particular embodiment, can be to soot stream
18 guide, and to be separated above and below drum 12 using exhaust, in other embodiments, only guide soot stream 18
To the side of drum 12.In addition, the speed for leaving the soot stream 18 of burner 16 can be relatively low, to be conducive to soot stream 18
It is first equably mixed before depositing on surface 14.In addition, burner 16 may include multiple outlet nozzles, and burner
16 can have the outlet nozzle of multiple small sizes, and the outlet nozzle of these small sizes, which plays, promotes soot stream 18 depositing to table
The effect first equably mixed before on face 14.In addition, burner 16 can be configured in the channel on the inside of burner more
Each ingredient and soot are mixed well, such as by Venturi nozzle and generate the flow guide for mixing and being vortexed.In some realities
It applies in mode, these structures can be formed by 3D printing.
In each embodiment, laser 24 is configured to the sheet glass 28 for further promoting to have smooth surface
It is formed.For example, in each embodiment, sintering laser 24 is configured to guide laser beam 26 to soot piece 20, with
Form sintering zone 36.In the embodiment shown, sintering zone 36 extends the entire width of soot piece 20.It is as follows will be more detailed
It discusses, laser 24 can be configured to control laser beam 26 in various ways to form sintering zone 36, so that sheet glass
28 have smooth surface.In each embodiment, laser 24 is configured to create the laser with certain energy density
Beam, the energy density are sintered soot piece 20 with the rate for forming smooth surface.
In each embodiment, the mean energy density of generated laser beam during sintering of laser 24 exists
0.001J/mm2To 10J/mm2Between, especially in 0.01J/mm2To 10J/mm2Between, more particularly in 0.03J/mm2To 3J/
mm2Between.In some embodiments, laser 24 may be particularly suited for being sintered thin soot piece (such as thickness be less than 200 μ
M, 100 μm, 50 μm etc.), in such an embodiment, the mean energy density for the laser beam that laser 24 generates exists
0.001J/mm2To 0.01J/mm2Between.
In other embodiments, system 10 is constructed, so that the opposite shifting between soot piece 20 and laser 24
The dynamic speed in favor of forming the sheet glass 28 with smooth surface occurs.In general, relatively fast on 22 direction of arrow
Degree is in 0.1mm/s between 10m/s.In each embodiment, relative velocity on 22 direction of arrow 0.1mm/s extremely
Between 10mm/s, especially in 0.5mm/s between 5mm/s, more particularly in 0.5mm/s between 2mm/s.In each implementation
In mode, system 10 is high speed sintering system, and relative velocity in the direction of arrow 22 is in 1m/s between 10m/s.
As shown in Figure 1, in one embodiment, laser 24 forms sintering zone 36 using dynamic beam shaping.?
In the embodiment, laser beam 26 is substantially scanned rapidly on soot piece 20 on the direction of arrow 38.Laser beam 26 it is rapid
Scanning simulates the linear laser beam of the substantially shape of sintering zone 36.In a particular embodiment, laser 24 utilizes two
Dimension galvanometer (galvo) scanner carrys out scanning laser beam 26, to form sintering zone 36.Due to using 2-D vibration mirror scanner, laser
Beam 26 can rasterize on the entire width of soot piece 20, or rasterize in the particular sub-area of soot piece 20.One
In a little embodiments, when soot piece 20 translates in the direction of arrow 22, laser beam 26 is rasterized.In the sintering process phase
Between, rasterisation speed can change according to required sintering characteristic and surface characteristics.In addition, the rasterization scheme of laser beam 26
Can be it is linear, sinusoidal, unidirectional, two-way, in a zigzag (zig-zag) etc., so as to generate have design and
The sheet material of selected flatness, density or other attributes.In such an embodiment, vibration mirror scanning can be used in laser 24
Device, polygon scanner, piezoelectric scanner and optical lasers beam-deflector, as AOD (acousto-optic deflection device) carrys out scanning laser beam 26
To form sintering zone 36.
In the specific embodiment for forming sintering zone 36 using the shaping of dynamic laser beam, with the speed of 1500mm/s
Bilateral scanning CO2Laser beam.CO2Laser beam has Gaussian intensity profile, 1/e2Diameter is 4mm.The step-length of bilateral scanning is
0.06mm.When setting sweep length is 55mm and laser power is 200W, substantially 400 μm of thickness of soot piece 20 is sintered
At the silica glass piece 28 with a thickness of~100 μm.Effective sintering velocity is~1.6mm/s, and sintering energy density is
0.65J/mm2。
In some embodiments, the shaping of dynamic laser beam and sintering method can be realized while scanning laser beam swashs
The modulated in real time of optical power.For example, controller can modulate sinusoidal power if scanning laser beam is distributed with sinusoidal velocity
Signal is sent to laser controller to maintain the constant laser energy density on soot piece 20 in sintering zone 36.
As shown in Fig. 2, in one embodiment, laser 24 carries out beam shaping using geometry/diffraction method with shape
At sintering zone 36.In this embodiment, laser 24 is used in combination elongated laser beam 26 to be converted into orthopedic systems 40
Laser beam 42.In each embodiment, orthopedic systems 40 may include one or more optical elements, for example, lens, prism,
Mirror, diffraction optical device etc., to form elongated laser beam 42.In each embodiment, elongated laser beam 42 is in soot piece
There is uniform intensity distribution along width direction on 20.In each embodiment, orthopedic systems 40 can be configured to
Width is generated in 1mm between 10m and highly in 0.5mm to the elongated laser beam 42 between 10mm.
It is formed in the specific embodiment of sintering zone 36 using geometry/diffracted laser beam shaping, utilizes Galileo
The CO that the beam expander extension diameter of design is 12mm2Laser beam.The diameter of laser beam by extension is about 50mm.Then it uses
Focal length is~the asymmetric non-spherical lens of 300mm will be converted by the laser beam of extension it is linear.The ruler of linear laser beam
Very little is 55mmx2mm.Laser power density is defined as laser power divided by area, is 1.8W/mm2.During sintering process,
Linear laser beam is remain stationary, while translating soot piece 20.When laser power is 200W, with the speed of 1.5mm/s by thickness
The silica glass piece 28 that substantially 400 μm of soot piece 20 sinters into a thickness of~100 μm.Corresponding sintering energy is close
Degree is 1.0J/mm2。
In each embodiment, laser 24 can be the laser with any wavelength or pulse width, as long as cigarette
Soot particle has enough absorptions to cause sintering.The absorption can be linearly or nonlinearly.In specific embodiment party
In formula, laser 24 is CO2Laser.In another embodiment, laser 24 can be wavelength and swash in 5 μm or so of CO
Light device.In such an embodiment, CO laser 24 can be deeper penetrated into soot piece 20, therefore CO laser 24 can
For being sintered thicker soot piece 20.In each embodiment, CO2The wearing in silica soot piece 20 of laser 24
Saturating depth is less than 10 μm, and the penetration depth of CO laser is~100 μm.In some embodiments, it can be preheated from rear side
Soot piece 20, for example, using resistance heater, IR lamp etc., to further increase the sintering depth formed by laser 24.
In some embodiments, system 10 is configured to the sintering temperature kept constant during laser sintered process
Degree.This can be realized by adding temperature sensor along sintering line.Temperature sensor data can be used for controlling laser function
Rate is to maintain constant sintering temperature.For example, a series of germanium or silicon detector can be installed along sintering line.Detector signal is by controlling
Device processed is read.Controller can handle these signals and correspondingly control laser output power using information.
With reference to Fig. 3, in one embodiment, laser 24, which can be configured to create, does not expand to soot piece 20
The sintering zone 36 of entire width.In some such embodiments, lesser sintering zone 36 can make neighbouring laser 24
And/or soot piece 20 occurs lower instrument and surprisingly heats.With reference to Fig. 4, in each embodiment, system 10 may include another
Outer laser 44 and 46, they are configured to completely or partially be sintered the marginal portion of soot piece 20.This can be advantageous
In the sheet material 28 for forming sintering in processing soot piece 20 of laser sintered period.
Unlike some silica glass forming technologies (such as ingot forming technology), system 10 is configured to
Generate the silica glass piece 28 with extreme high purity level and extremely low thickness.In each embodiment, silica glass
The thickness (that is, perpendicular to size of main surface and subsurface) of glass piece 28 less than 500 μm, less than 250 μm, less than 150 μm and
Less than 100 μm.In addition, silica glass piece 28 is the silica of at least 99.9 moles % in each embodiment, it is special
It is not the silica of at least 99.99 moles %.In addition, the silica glass piece 28 formed has the pollutant of extremely low level
Element, these pollutant elements are common in the silica glass formed by other methods.In specific embodiment party
In formula, total sodium (Na) content of silica glass piece 28 is less than 50ppm.In each embodiment, silica glass piece
28 sodium content is substantially coincident in entire sheet material 28, so that total sodium of all depths in silica glass piece 28
Content is respectively less than 50ppm.This low total sodium content and the distribution of uniform sodium and some silicon dioxide structures (such as titanium dioxide
Silicon ingot material) comparison is formd, these silicon dioxide structures are at the different depth with higher total sodium content and in ingot
Variation.In each embodiment, it is believed that discussed herein low compared to other earth silicon materials with higher sodium content
Sodium content provide reduced with optical loss, the sheet glass 28 of index of refraction homogeneity and chemical purity/non-reacted.
In other embodiments, silica glass piece 28 has low-level hydroxyl (OH) concentration.In each implementation
In mode, OH concentration can control, to influence the viscosity of silica glass piece 28, refractive properties and other properties.Each
In a embodiment, β-OH is less than 0.02abs/mm, more specifically, being less than 0.02abs/mm.In some embodiments, it utilizes
Laser sintering system 10 formed silica glass piece 28 OH concentration be less than using some other manufacturing process (such as etc. from
Daughter sintering, flame sintering and/or first using the dry sintering process being sintered again of chlorine) OH of earth silicon material that is formed
Concentration.It is contrasted with some earth silicon materials being surface-treated using certain substance (such as hydrofluoric acid), two
Silica glass piece 28 has low surface halogen concentration and low surface OH concentration.
In each embodiment, the fictive temperature (Tf) of the silica glass piece 28 through oversintering is more at least above
The Tf of earth silicon material (such as silica ingot).Such as, it is believed that at least in some embodiments, two through oversintering
The fictive temperature of silica glass piece 28 is more special especially between 1500 DEG C to 1800 DEG C between 1100 DEG C to 2000 DEG C
It is not between 1600 DEG C to 1700 DEG C.In a specific embodiment, silica glass piece 28 through oversintering
Fictive temperature is about 1635 DEG C (such as 1635 DEG C of increases and decreases 1%), such as this glass of full annealing.
With reference to Fig. 5-8C, the surface profile of the sheet glass 28 through oversintering is shown according to illustrative embodiments, is opened up
It flutters and roughness features.Fig. 5 shows the reality of the silica glass piece 28 formed using the scanning laser system based on galvanometer
Apply the Zhai Ke optical profile scanning situation of mode (such as embodiment shown in FIG. 1).Fig. 6 is shown to be swashed using geometry/diffraction
Beam shaping and the Zhai Ke optics wheel of the embodiment (such as embodiment shown in Fig. 2) of silica glass piece 28 formed
Exterior feature scanning situation.Fig. 7 is according to an illustrative embodiments, and the surface of the embodiment of silica glass piece 28 measures
The 3D minute yardstick schematic diagram of profile.Fig. 8 A-8C shows the length along sheet glass 28 shown in Fig. 7, in three different locations
The atomic force microscope line for locating the surface of the silica glass 28 of taken transverse scans situation.
In each embodiment, the sheet glass 28 through oversintering has opposite the first main surface and the second main surface,
At least one main surface therein has high smoothness level.In each embodiment, the first of the sheet glass 28 of sintering
The roughness (Ra) of at least one of main surface and the second main surface is at least one 0.023mm2In area 0.025nm extremely
Between 1nm, especially in 0.1nm between 1nm, and especially in 0.025nm between 0.5nm.It is real as one
It applies in mode, determines Ra using Zhai Ke optical profilometry shown in Figures 5 and 6, be 130 μ especially with spot size
Mx180 μm of Zhai Ke instrument determines.In some embodiments, the first main surface of the sheet glass 28 of sintering and the second main table
The roughness (Ra) at least one of face is in 0.12nm between 0.25nm, this in 2 μm of line scannings using AFM by being surveyed
, as shown in figures 8 a-8 c.In a particular embodiment, the sheet glass 28 of sintering is when small scale is measured with low coarse
Degree is horizontal, has biggish roughness levels in large scale measurement.In each embodiment, the sheet glass 28 of sintering
The roughness (Ra) of at least one of first main surface and the second main surface is at least one 0.023mm2In area
0.025nm uses the Ra when sweep length of contourgraph and 5mm with 1 μm to 2 μm between 1nm.
As shown in Fig. 5-8C, although sintering sheet glass 28 each main surface be it is smooth, these surfaces have really
There is a series of Nanoscale Surface topology comprising protrusions and recess feature.In embodiment discussed herein, protrusion and recess
Feature is relatively small, is conducive to low surface roughness.Average height or baseline in each embodiment, relative to topology
Highly, the maximum peak heights of each protruding features are between 0.1 μm to 10 μm, and especially between 1 μm to 2 μm, this uses wheel
The sweep length of wide instrument and 5mm measures.In a particular embodiment, the topological feelings on one or more surfaces of sheet glass 28
Condition is at least one 0.023mm2In area, the top at the bottom of recess feature (such as paddy) and protruding features (such as peak) it
Between maximum normal distance in 1nm between 100nm, this is measured by Zhai Ke optical profilometry.Table 1, which is shown from one, to be shown
The coarseness data that the AFM scan situation on the surface of the sheet glass 28 of the sintering of example property embodiment obtains.
Table 1
If Fig. 7 is best shown, silica glass piece 28 may include multiple gaps or bubble.In each embodiment
In, some of which gap or bubble can be located on the surface of silica glass piece 28, to form recess shown in Fig. 7
50, and other bubbles or gap can be located at the interior zone of the earth silicon material through oversintering of silica glass piece 28
It is interior.In this embodiment, bubble or gap make two of the bulk density of sheet material 28 less than the sintering of tight or bubble
The maximal density of silica.In each embodiment, the silica glass piece 28 of sintering is fully sintered silica
Piece (such as with sheet materials a small amount of or without unsintered silica soot particles), density are greater than 1.8g/cc and are less than
2.2g/cc, especially less than 2.203g/cc (such as the fully sintered silica without any gap or bubble is most
Big density).In such an embodiment, the initial density of soot piece 20 can in 0.2g/cc between 0.8g/cc, and
By the interaction with laser beam 26, soot piece 20 is fine and close to be melted into fully sintered silica glass piece, and density is greater than
1.8g/cc and be less than 2.203g/cc, specifically between 1.8g/cc to less than 2.15g/cc.In each embodiment,
The formation of bubble, gap or surface concave 50 can be controlled by control laser operations, can also be by by from soot burnt
Device 16 travels out the particle matter impact come and is formed.In each embodiment, the gap in silica glass piece 28 is (outstanding
It is recess 50) it can be advantageous in the application for example for the substrate of carbon nanotube (CNT) growth, wherein recess 50 is used
In holding CNT catalyst.
In order to be compared, Fig. 9 shows the silica ingot 60 by polishing formed by non-laser sintering process,
Especially from the Zhai Ketu of the sliced of titanium dioxide silicon ingot and polishing part.As shown in figure 9, the titanium dioxide silicon ingot by polishing
The surface topology of material 60 has different from the surface topology of different embodiments of sheet glass 28 of sintering shown in Figures 5 and 6
Appearance.For example, ingot 60 has linear abrasion label 62, may be formed during the different step of ingot formation process, example
As formed during processing and/or during polishing.In addition, the surface topology of ingot 60 shown in Fig. 9 has directionality, wherein table
Region feature extends generally on the moving direction of burnishing device and (extends from the upper left corner shown in figure to the lower right corner).On the contrary, Fig. 5
With 6 shown in the surface topology of embodiment of silica glass piece 28 show the distribution of more random peak and valley, and
And almost without directionality.In such an embodiment, silica glass piece 28 does not include elongated raised or sunken spy
Sign, wherein at least one 0.023mm2In area, the maximum length and maximum width of protrusion and/or recess feature are less than 10 μ
M, especially less than 3 μm, in some embodiments, less than 1 μm.
In some embodiments, silica glass piece 28 can have body curvature or warpage, so that silica glass
Each corresponding main surfaces of glass piece 28 are offset slightly from planar configuration.As shown in figures 8 a-8 c, in some embodiments, silica
One of main surface of sheet glass 28 has spill, extends on the width of sheet material 28, so that wherein the one of sheet material 28
The center of a main surface is lower than the side edge of sheet material 28.In each embodiment, when in 3750mm2Area in measurement when,
The warpage of sheet material 28 is in 0.5mm between 8mm.In an example, with only moral on the sheet material 28 having a size of 50mmx75mm
(Werth) measuring instrument measures and obtains the warpage situation of the sample of sheet material 28.In another embodiment, exist
The warpage of sheet material 28 is measured on the rectangular area of 150mmx150mm less than 20 μm.
In each embodiment, there are two main surfaces for the tool of silica glass piece 28, and upper surface is by towards soot burnt
The part of the soot piece 20 of device 16 is formed, and lower surface is formed by the part of the soot piece 20 of contact drum 12.In each embodiment
In, any one of upper surface or lower surface of silica glass piece 28 or both of which can have discussed herein any
Feature.In a particular embodiment, the upper surface of silica glass piece 28 can have surface characteristics discussed herein, under
Surface has surface structure, topology, roughness, the surface chemistry etc. different from upper surface because contacting with drum 12.Have at one
In the embodiment of body, the roughness (Ra) of the lower surface of titanium dioxide silicon wafer is greater than the roughness of upper surface, silica glass
The Ra of the lower surface of piece 28 can be between 0 μm to 1 μm.In another embodiment, the lower surface of titanium dioxide silicon wafer 28
Roughness (Ra) is less than the roughness of upper surface, in such an embodiment, to soot deposit surface after removing soot piece
(such as surface 14 of drum 12), which carries out cleaning, can make the lower surface of silica piece 28 have high-caliber smoothness.
In each embodiment, can control laser 24 in various ways to be formed has different characteristic, layer and/or table
Face structure fully sintered or the sheet glass 28 partially sintered.Since porous bodies (such as soot piece 20), burnt by changing
Knot condition can obtain different porosity and/or surface topology in the sheet material being partially or fully sintered.In an embodiment party
In formula, CO2Laser heat source forms narrow sintering region, can be used for controlling porosity and surface topology.In each reality
Apply in mode, sintering velocity, laser type and laser power combination can various features (such as the material based on soot piece 20
Expect type, thickness, density etc.), the requirement of the product of the sheet material 28 based on sintering to be utilized, and/or wanted based on downstream process
It asks and changes.In each embodiment, above system 10 can be operated to form the sheet material 28 of the sintering with various features.
It, can (such as opposite between soot piece and laser be moved with the sintering velocity of 0.5mm/s to 5mm/s in each embodiment
Dynamic speed) operating system 10, laser 24 can be the CO that power is 100W to 300W2Laser.In some embodiments,
Soot piece 20 is primary by the laser sintered region of laser 24, in other embodiments, 20 multipass laser of soot piece
The laser sintered region of device 24.
Figure 10 provides the example for the different structure that can be formed under different sintering conditions.Such as the top lattice institute of Figure 10
Show, the sheet glass partially sintered with speckled surface structure, which can use, generates elongated laser beam (such as light beam 42 of Fig. 2)
100W CO2The sintering bulk density of laser 24 is 500 microns of soot pieces 20 of 0.35g/cc to be formed, wherein sintering velocity
(such as relative moving speed between soot piece and laser) is 0.65mm/s.As shown in the middle layout of Figure 10, having more has
Tissue and the sheet glass of linear surface structure partially sintered can use 200W CO2Scan laser 24 (such as above for
Described in Fig. 1) sintering bulk density be 0.35g/cc 500 microns of soot pieces 20 formed, wherein sintering velocity (such as soot piece
Relative moving speed between laser) it is 1.3mm/s.It is fully sintered with smooth surface as shown in the bottom sieve frame of Figure 10
Sheet glass (as discussed herein) can use 300W CO2It is 0.35g/cc's that scan laser 24, which is sintered bulk density,
500 microns of thick embodiments of soot piece 20 are formed, and wherein sintering velocity is (such as opposite between soot piece and laser
Movement speed) it is 1.95mm/s.
In addition, in each embodiment laser 24 can be controlled in various ways to form fully sintered or part and burn
The sheet glass 28 of knot, in the sheet glass 28 partially sintered, the soot piece 20 of only a part is sintered, so that the titanium dioxide of sintering
Silicon layer is supported by unsintered soot lower layer.In each embodiment, it can first be moved before using silica sinter layer
Except remaining soot layers, in other embodiments, remaining soot layers can remain together with silica sinter layer.
In each embodiment, it is fully sintered to be formed in the part of unsintered soot that laser 24 can be controlled in various ways
Structure.In some embodiments, sintering column and/or hollow sintered pipes can be formed in soot piece 20.
In some embodiments, the silica glass piece 28 of sintering is by least 99.9 weight %, especially at least
The group of 99.99 weight % becomes (SiO2)1-x-y.M′xM″yMaterial constitute, wherein any one in M ' and M " or two kinds are member
Plain (such as metal) dopant replaces form, can be in oxide form perhaps their combination or M ' and M "
Any one or two kinds be omitted, and for any one of M ' and M " or two kinds, x adds the sum of y less than 1, is, for example, less than
0.5 or x and y is 0.4 or smaller, such as 0.1 or smaller, such as 0.05 or smaller, such as 0.025 or smaller, and one
In a little such embodiments, it is greater than 1x10-6.In some embodiments, the silica glass piece 28 of sintering is crystal,
In some embodiments, the silica glass piece 28 of sintering is amorphous.
In each embodiment, the silica glass piece 28 of sintering is firm and flexible substrate, can be with
Allow the device made of sheet material 28 that there is flexibility.In each embodiment, the silica glass piece 28 of sintering is bendable
It is bent so that when at 25 DEG C at room temperature, wafer warpage at least radius of curvature of 500mm and it is not broken.Specifically implementing
In mode, the silica glass piece 28 of sintering is flexible, so that when at 25 DEG C, at room temperature, wafer warpage is at least
The radius of curvature of 300mm and it is not broken, more specifically, when at 25 DEG C at room temperature, wafer warpage at least curvature of 150mm partly
Diameter and it is not broken.The bending of the titanium dioxide silicon wafer 28 of sintering can also be conducive to the application of reel-to-reel, such as set in automated manufacturing
Across roller processing in standby.
In each embodiment, the silica glass piece 28 of sintering is the transparent or semitransparent of silica glass
Sheet material.In one embodiment, transmissivity (such as the transmission in the visible spectrum of the silica glass piece 28 of sintering
Rate) it is greater than 90%, more particularly greater than 95%.In each embodiment, the silica glass piece of sintering discussed herein
Softening point temperature be greater than 700 DEG C.In each embodiment, the silica glass piece of sintering discussed herein about 50 to
There is the low thermal expansion coefficient less than 10 × 10-7/ DEG C within the temperature range of 300 DEG C.
Although other sintering equipments can be used to implement some embodiments, applicant have discovered that with disclosed herein
Ad hoc fashion carries out laser sintered advantage.For example, it is found by the applicant that laser sintered can damage surrounding instruments with non-radiating
Heat, the cause thermal damage surrounding instruments of radiation may be by induction heating and resistance heating be sintered there are the problem of.Applicant
It was found that laser sintered have good temperature control and temperature repeatability, and sheet material 28 can not be made to be bent or with other
Mode warpage, sheet material 28 bending or otherwise warpage may be flame sintering there are the problem of.Compared to these other works
Skill, it is laser sintered required heat to be supplied directly to and only be supplied to the part for needing the soot piece being sintered.Laser
A large amount of pollutant and gas can not be sent into sintering zone by sintering, and a large amount of pollutant and gas may interfere with fine sheet
Manufacture.In addition, it is laser sintered can also dimensionally extend or speed increase.
In each embodiment, silica soot piece disclosed herein is raw by using one or more glass soots
It is formed at the system of device (such as flame hydrolysis burner), described device is intended to or is intended to for glass soot particles stream being transmitted to
On soot deposit surface.As described above, titanium dioxide silicon wafer discussed herein may include one or more dopants.In flame water
In the example for solving burner, doping can be in situ during flame hydrolysis process and dopant precursor is introduced into flame
Occur.In additional examples, it such as in the case where the soot sprinkler of plasma heating, is sprayed from sprinkler
Soot particles can be pre-doping, alternatively, the soot particles sprayed can be made to be subjected to the plasma atmosphere containing dopant,
Soot particles to be adulterated in the plasma.In additional examples, it can will be adulterated before or during being sintered soot piece
Agent covers in soot piece.Illustrative dopant includes IA race, IB race, Group IIA, Group IIB, IIIA in the periodic table of elements
Race, IIIB race, IVA race, Group IVB, VA race, VB race element and rare earths.In each embodiment, silica soot
Grain can be doped with various substances, including germanium oxide, titanium dioxide, aluminium oxide, phosphorus containg substances, rare earth element, metal and fluorine.
Embodiment 1
400 be made of using the preparation of method described in No. 7,677,058 United States Patent (USP) substantially 100% silica
The thick soot piece of micron.The 9 inches wide soot piece for multiplying 12 inches long is partially disposed in CO2On translation stage near laser.
The laser is the 400W CO of the model E-400 purchased from relevant company (Coherent Inc.)2Laser.In laser
Asymmetric non-spherical lens is placed between soot piece.The asymmetric non-spherical lens generates 10mm long and about 1mm's wide
Line beam, and uniform intensity distribution is all had on long axis and short axle.Lens are placed on the position from soot agreement that contracts a film or TV play to an actor or actress 380mm
Set place.The power that the laser power used is 18 watts.Soot piece moved past light beam with 1.25mm/ seconds.It is formed in beam path
Complete densification, transparent sintered glass.When soot be densified and shrink separated with remaining soot piece when, sintering
Sheet material has wonderful low amount of distortion.In other sintering systems, soot sector-meeting bending and deformation, unless in sintering process
Period lies in soot piece in a certain plane.
Embodiment 2
Other than with 1.5mm/ seconds translation soot pieces, embodiment 2 is same as Example 1.This is on unsintered soot piece top
The glassy layer of part densification is produced in portion.
Embodiment 3
In addition to the substantially 100% silica soot piece by solute doping with when with laser sintered in silica
It is provided in matrix outside a small amount of Yb doping, embodiment 3 is same as Example 1.
The different reason of fictive temperature may be according to the fusing of method disclosed herein laser 114 and cooling marginal portion
112 may with for heat/process of the remainder of cooling sheet material 110 is identical, this is enough to establish " fingerprint ".For example, from
Cut down in ingot and then with laser cutting with formed the thin silicon dioxide piece of marginal portion as described herein mass center with
The fictive temperature of edge surface may have particularly apparent difference.Toughness and crackle, which mitigate performance, to be influenced by fictive temperature
And/or it is associated, wherein different heat treatment can provide better performance.
* * *
By ring test on empirical ring, applicants have discovered that evidence show laser sintering process disclosed herein relative to
The Normal silica piece for cutting down and polishing from ingot can improve the intensity of corresponding thin silicon dioxide piece.Application
People thinks that this may be because by silica on piece as disclosed herein manufactured by method disclosed herein, not depositing
Or eliminate residual stress and/or face crack present in ingot cutting sheet material and cause site.
Applicant further found that specific laser movement patterns, setting condition and/or behaviour can be used during sintering process
Make condition, to obtain the particular surface attribute of high purity fused silica piece disclosed herein.For example, the line of laser beam scans
The peak and valley to rise and fall can be generated along corresponding titanium dioxide silicon chip surface, and quickly polygon raster display can produce micro- saw
Tooth, as described below.
It with reference to Figure 11-13, is sintered using line scanning laser, is produced by silica soot piece with a thickness of 500 μm or lower
Thin high purity fused silica piece 310.The sheet material 310 includes peak 312 and the paddy of the fluctuating along corresponding sheet glass 310
314.As that can see from two dimensional plot, each peak 312 near paddy 314 is spaced from each other a distance, which is at least
It 1000 μm, for example, at least 2000 μm, at least 4000 μm, is measured from the top at each peak 312.Paddy relative in adjacent each peak compared with
The depth D of the height of high person is at least 1 μm, for example, at least 1.5 μm, at least 2 μm.Along the small protrusion on the surface between adjacent peak
Local peaks are different from, because their amplitude is much smaller, that is, except the D range.Each peak and valley 312,314 along
The surface longitudinal of sheet material 310 extends at least distance of 1mm (see, for example, the horizontal direction in Figure 11, the direction of slice 1 and 2),
For example, at least 5mm or bigger distance, this is for example depending on the size and other factors of sheet material 310.
As that can see from Figure 11-13, sheet material 310 further includes the ditch for being typically normal to the length of peak and valley 312,314
316.Although peak and valley 312,314 is attributed to laser sintered pattern by applicant, ditch line is attributed to and is used for shape by applicant
At the variation of the width of the silica soot piece of high purity fused silica piece.In the process for forming silica soot piece
Period, the soot stream from hydrolytic process may make soot correspond to the depth deposition near each local nozzle, this may be
It is non-uniform.This results in ditch 316, as shown in figure 12.
Although the sheet material 310 of Figure 11-13 is manufactured using line scanning laser sintering process, other realities of the disclosure
The mode of applying is related to a kind of method for being sintered high purity fused silica glass piece 410, and the method includes in high-purity consolidation
Silica soot on piece rasterizes the step of laser beam;The pattern wherein rasterized includes the tight spacing on sheet material 410
Target position when observing on section, makes laser sintered soot and forms micro- saw in the first main surface of sheet material 410 simultaneously
Tooth.As it is used herein, rasterisation refers to the general scanning motion on the laser beam surface for sintering, such as with phase
To the form of movement, for example, it is general move forward and backward, polygonal spiral circulatory motion etc..In some embodiments, it rasterizes
Pattern includes moving laser beam with generally polygonal shape, wherein the vertex of polygonal shape is sphering.For example, titanium dioxide
Silicon wafer 410,610 is manufactured with this laser sintering process.
Figure 14 conceptually illustrates surface 510 and the corresponding small recess 550 and coronal of sheet glass disclosed herein
Object 552, for the crown 552 near recess 550 and between each recess 550, the sheet glass can be by being disclosed herein
Sintering method and technology production.There is each small recess 550 depth D1, the depth D1 nominal contour measuring method, phase can be used
The higher person in adjacent crown 552 on the either side of recess 550 is measured.For example, in titanium dioxide silicon wafer 410,610
On this small recess depth D1 be at least 25nm and be no more than 1 μm.
According to an illustrative embodiments, the recess 550 is zigzag or forms " micro- sawtooth ", so that at least one
A little bottom surfaces of the recess with general planar and at least some corresponding adjacent crowns have the top surface of substantially platform, institute
The top surface for stating substantially platform is deviateed by the side wall at steep angle with bottom surface.Recess 550 corresponds to the bottom of micro- sawtooth
Surface, and crown 552 corresponds to top surface.The surface of recess 550 and crown 552 can change because of the angle of respective surfaces
Become and be different from the side wall of top surface and bottom surface edge, wherein meaning " at steep angle ", if bottom surface and/or top table
Face is substantially aligned with horizontal plane, then side wall and the plane differed within 30 degree with vertical line are substantially aligned.
With reference to Figure 15-17, titanium dioxide silicon wafer 410 includes small recess 412, and the depth of each small recess 412 is no more than
500nm, the depth are measured relative to the higher person in the adjacent local crown on the either side of respective notches 412.Root
According to an illustrative embodiments, width of each recess 412 between adjacent local crown is at least 5 μm but is no more than
500μm.In some embodiments, width of each recess 412 between each local crown is at least 50 μm.Each recess 412
Length be at least 500 μm, for example, at least 1000 μm, as shown in figure 14 (horizontal direction, the direction of slice 1 and 2).In some realities
It applies in mode, the length of each recess is at least 2500 μm.
According to an illustrative embodiments, micro- sawtooth 414 gathers to form elongated column 414 along surface side by side.
The size of elongated column 414 is limited by the outmost recess 412 in corresponding set, wherein adjacent recesses 412 in set it
Between distance D2 (referring generally to Figure 14) measured according to the depth capacity of each recess 412, the distance D2 be no more than 500 μm, example
Such as it is no more than 300 μm and/or be at least 25 μm, for example, at least 50 μm.According to an illustrative embodiments, elongated column
414 be at least 1mm wide and 2mm long, and elongated column 414 include the small recess 412 of at least ten.In some embodiments, carefully
Long line 414 includes at least 15 small recess 412.
In some such embodiments, the pattern of micro- sawtooth makes when observing sheet material 410 in cross-section, at least
Three recesses 412 abreast define rows each other, and the depth of each recess 412 differs 20% with the mean depth of three recesses 412
Within and/or adjacent recess 412 as at least five, depth differed within 20% with the mean depth of five recesses.
The size and geometrical homogenization of recess 412 can indicate the method for manufacturing corresponding sheet material 410, and relative to less
Uniform sheet material, the method can make the consistency of performance of sheet material 410 and predictable be improved.
Compare the micro-structure of Figure 11-13 and Figure 15-17, the crown and recess 412 of sheet material 410 are in each surface characteristics
General proportion and vpg connection are different from peak 312 and paddy 314.Micro- sawtooth is usually tooth form, and has substantially sharp and/or saw
The side of dentation (referring generally to the recess 550 and crown 552 of Figure 14).Recess 412 and crown often have flat or water
Flat surface, and peak and valley 312,314 be it is smooth rise and fall and sphering without interruption, edge, angle.These differences may be by
In apply during sintering process laser beam as described above it is different caused by.
It has been found that it is close place formed as disclosed herein micro- sawtooth recess 412 can cover and/or remove by
It is sintered ditch caused by the soot piece with non-uniform soot deposit object (for example, see the ditch 316 of Figure 11).It is some in this way
Embodiment in, obtained result may be wavy less big surface and substantially more flat geometry.In addition, using
The rasterisation of polygon beam pattern can remove the rigidity source of sheet material to generate micro- sawtooth by removal ditch, thus enclosing
It can make flexible improvement when around the bending shaft being aligned with micro- sawtooth, especially if micro- sawtooth is extended approximately along straight line path
When.
In other embodiments, the small recess 412 of micro- sawtooth is along its curved in length, it means that recess is along bending
Path longitudinally extend.For example, in some such embodiments, curve and straight line deviate at least 10 degree (see, for example, figure
14 curve C).In some embodiments, it remains along and turns in the recess 412 of micro- sawtooth of the approximate location of this turning point
It is separated from each other to place, it means that recess 412 will not usually be assembled each other.In some embodiments, along the recessed of micro- sawtooth
The curve in the path of mouth 412 includes at least 90 degree of turning point.In some embodiments, curve is usually formed with sphering
The polygon on vertex.In other embodiments, recess is not bent, or can have the part of curved notches by cutting off
Curve is removed from sheet material.
With reference to Figure 18-20, high purity fused silica glass piece 610 is at least the silica of 99.9 moles of %,
Middle silica is at least generally amorphous, thus has the crystalline content less than 1 weight %.Sheet material 610 is in each main surface
Between average thickness less than 500 μm.As shown in figure 19, when observing in cross-section, main surface has along main surface
Small recess 612.The depth of each small recess 612 be at least 25nm but be no more than 1 μm, either side of the depth relative to respective notches
On adjacent local crown in the higher person measure.Width of each small recess between adjacent local crown is at least
5μm.The length of each small recess is at least 500 μm.It is not " recess " of sheet material 610 without those of these attributes feature.Such as figure
Shown in 19, recess is zigzag, so that at least some recesses have the bottom surface of general planar and at least some corresponding adjacent
Crown has the top surface of substantially platform, and the top surface of the substantially platform passes through the side wall and bottom table at steep angle
Deviate in face.
Referring now to Figure 18, applicant thinks that high purity fused silica has for the excellent of the substrate in electronic device
Good attribute, because it is with relevant dimensional stability and dielectric property and other attributes, so that electronic device be allowed to become more
It is compact and energy saving.However, it is possible to be difficult to for metal layer to be integrated to Normal silica on piece, because of their own coefficient of thermal expansion
Variant, this is layered after can lead to temperature change.In Figure 18, electronic device 810 (such as printed circuit board, antenna or
Other similar device) it include substrate 812 (such as interpolater, plate), which includes high-purity consolidation dioxy disclosed herein
SiClx sheet glass 814.
In some such embodiments, high purity fused silica piece 814 has micro- sawtooth in main surface 818
816.Micro- sawtooth 816 can be useful due to various reasons, for example, promote or reinforce with thin conductive layer 820 (for example, comprising
Copper, aluminium, gold metal) combination, such as by increase interfacial surface area and/or with the orthogonal arrage area at interface, this can subtract
Gently layering effect caused by the shearing force due to caused by the different heat expansion rate from titanium dioxide silicon wafer 814 and conductive layer 820.
Conductive layer 820 can be sputtered or otherwise be deposited on substrate, so that partial electroconductive layer 820 is filled into micro- saw
In the recess of tooth 816.It is knitted according to the downside of illustrative embodiments, the conductive layer 820 towards micro- sawtooth 816 with certain pattern
Structure, the geometry inverse correlation of the pattern and micro- sawtooth 816 make the crown on main surface 818 correspond to conductive layer 820
Downside on recess, and the recess on the downside of conductive layer 820 correspond to main surface 818 on crown.
Although substrate 812 is shown in Figure 21 as high purity fused silica glass piece 814, in other imaginations
Embodiment in, high purity fused silica glass piece 814 can be coated with another material, for example, adhesion promotor or
Material with intermediate thermal expansion property is to promote the combination between high purity fused silica piece 814 and conductive layer 820.Cause
This, the metal layer 820 of electronic device 810 is connected to substrate 812 and covers micro- sawtooth 816, and conductive layer 820 can be directly or logical
It crosses middle layer and is connected indirectly to substrate 812 and/or high purity fused silica glass piece 814.
According to an illustrative embodiments, the thickness of Bao Jicai 812 and/or high purity fused silica glass piece 814
Spending T is 1000 μm or smaller, such as 500 μm or smaller, such as 200 μm or smaller.It is high-purity according to an illustrative embodiments
The porosity of fused silica silicon wafer 814 is spent less than 10 volume %, is, for example, less than 5%, is, for example, less than 2%.Imagine at other
In embodiment, high purity fused silica piece 814 has bigger porosity.Wherein hole, which corresponds to, is not present titanium dioxide
Silicon but gap, gap or the bubble that may exist gas or other materials.
Applicant thinks can be with along the curvature C (referring to Figure 15) of the length of recess 412,612 and corresponding micro- sawtooth 816
Improve the knot on the surface 818 of material (such as conductive layer 820 or coating or other materials) and titanium dioxide silicon wafer 410,612,814
It closes, this in main surface 818 by providing surface characteristics, and these surface characteristics and the multiple directions along main surface 818
Shearing force on the contrary, such as surface characteristics opposite with only straight micro- sawtooth is realized.
Applicant have observed that in some applications or on the way, fused silica glass piece 110 disclosed herein and other
Substance can be coated with other material, these materials can not be silica, and/or can combine or with its other party
Formula is connected to other or different material.In the embodiment of some imaginations, sheet glass identical with sheet material 110 has at least
The group of 99 weight % becomes (SiO2)1-x-yM′xM″yGlass, wherein any one in M ' and M " or two kinds be element, doping
Agent replaces form, can be any one in oxide form perhaps their combination or M ' and M " or two kinds
Be omitted, and x adds the sum of y less than 1, be, for example, less than 0.5 and/or x and y be 0.1 or smaller, such as 0.05 or smaller, for example
0.025 or smaller, and in some such embodiments, for any one of M ' and M " or two kinds, x and y are greater than 10
×10-7。
In the embodiment of imagination, in addition disclosed titanium dioxide silicon wafer can be described to mix doped with dopant herein
Miscellaneous dose includes IA race, IB race, Group IIA, Group IIB, Group IIIA, IIIB race, IVA race, Group IVB, VA race, VB in the periodic table of elements
The element and/or rare earths of race, such as be doped by the way that dopant precursor to be introduced into flame hydrolysis burner.It is setting
In the embodiment thought, sheet glass as described herein has the SiO of at least 50 moles %2, can be with other elements or molecule
Mixture, the SiO of for example, at least 70 moles %2Or the SiO of 90 moles of %2。
In some embodiments, high purity fused silica is amorphous, as used herein, it means that it has
There is the crystalline content no more than 1 weight %.In the embodiment of some imaginations, the sheet material can be crystalline quartz and/or
Glass ceramics, crystalline content are for example, at least 1 weight %.
* **
Unless otherwise stated, it is otherwise all not intended to and is interpreted as any means as described herein to need to make its step with specific
Sequence carries out.Therefore, it is set fourth as that its step follows certain sequence or it does not exist when claim to a method is practically without
It specifically indicates that step is limited to specific sequence in claims or specification with any other modes, is all not intended to imply that this
Meaning particular order.In addition, as it is used herein, article "one" be intended to include one or more than one component or element, and
And it is not intended to and is understood to mean only one.
It will be apparent to those skilled in the art various modifications can be carried out and changes without departing from open
Embodiment spirit or scope.Because those skilled in the art can be public to institute in conjunction with the spirit and essence of embodiment
The embodiment opened carries out various improvement, combination, subitem combination and variation, therefore, it is considered that embodiment of the present disclosure includes
Full content and its equivalent in scope.
Claims (20)
1. a kind of high purity fused silica glass piece, includes:
First main surface;
Second main surface opposite with the first main surface;
The silica of at least 99.9 moles %, wherein the silica is at least generally amorphous, to have less than 1 weight
Measure the crystalline content of %;And
The average thickness less than 500 μm between the first main surface and the second main surface;
Wherein, in cross-section, the first main surface has the small recess along the first main surface, wherein at least ten small recesses
It includes
At least 25nm but the depth no more than 1 μm, the depth is relative to the adjacent local crown on the either side of respective notches
In the higher person measure,
At least 5 μm of the width between adjacent local crown, and
At least 500 μm of length.
2. high purity fused silica glass piece as described in claim 1, wherein the recess is zigzag, so that extremely
Few some recesses have the top table of usually platform with the bottom surface and at least some corresponding adjacent crowns being generally flat
Face, the top surface are deviateed by the side wall at steep angle with bottom surface.
3. high purity fused silica glass piece as described in claim 1, wherein the small recess of at least ten is main along first
Surface respectively differs within 1000 μm at least one other small recess, and at least three recesses line up one side by side each other
Row, the depth of each recess differ within 20% with the mean depth of three recesses.
4. high purity fused silica glass piece as described in claim 1, wherein small recess is along its curved in length.
5. high purity fused silica glass piece as claimed in claim 4, wherein the curve of small recess is deviated to straight line
It is 10 degree few.
6. high purity fused silica glass piece as claimed in claim 5, wherein curve exists along the length of small recess
At least 10 degree are turned in 500 μm of distance but are no more than 360 degree.
7. high purity fused silica glass piece as claimed in claim 6, wherein each small recess at steering position along
Turning point maintains separately from each other.
8. high purity fused silica glass piece as claimed in claim 6, wherein small recess along the length of small recess with
The form continuously turned to is bent at least 90 degree.
9. high purity fused silica glass piece as claimed in claim 6, wherein the curve is generally formed with sphering
The polygon on vertex.
10. high purity fused silica glass piece as claimed in claim 6, wherein each recess each local crown it
Between width be at least 50 μm, and the respective depth of small recess be at least 100nm but be no more than 500nm, the depth
Relative to the higher person measurement in the adjacent local crown on the either side of respective notches.
11. high purity fused silica glass piece as claimed in claim 10, wherein the length of each recess is at least 2500
μm。
12. a kind of electronic device comprising:
Thin substrate, it includes with a thickness of 500 μm or smaller high purity fused silica piece, wherein the high-purity consolidation
Titanium dioxide silicon wafer includes recess in its main surface, wherein the recess is zigzag, so that at least some recesses have generally
For flat bottom surface and at least some corresponding adjacent crowns have the top surface of generally platform, and the top surface passes through
Deviate at the side wall and bottom surface of steep angle;With
Metal layer connect with thin substrate and covers recess, wherein is textured on the downside of the metal layer towards sawtooth a certain
The geometry inverse correlation of pattern, the pattern and sawtooth, so that the crown in the main surface of high purity fused silica piece
Corresponding to the recess on the downside of metal layer, and the recess on the downside of metal layer corresponds to the high-purity fused silica of substrate
Crown in the main surface of silicon wafer.
13. electronic device as claimed in claim 12, wherein the recess is small recess, and the depth of each recess is at least
25nm and it is no more than 1 μm, the depth is surveyed relative to the higher person in the adjacent local crown on the either side of respective notches
Amount, wherein each recess has the width for being at least 5 μm between adjacent local crown, and the length of each recess is at least
500μm。
14. electronic device as claimed in claim 13, wherein metal layer directly contacts thin substrate.
15. electronic device as claimed in claim 14, wherein metal layer directly contacts the high-purity fused silica of thin substrate
Silicon wafer.
16. electronic device as claimed in claim 12, wherein Bao Jicai with a thickness of 200 μm or smaller.
17. electronic device as claimed in claim 12, wherein the porosity of high purity fused silica piece is less than 10 bodies
Product %.
18. a kind of sintering is with a thickness of 500 μm or the method for smaller thin high purity fused silica glass piece, the method
It is included in the step of high purity fused silica soot on piece rasterizes laser beam, wherein the pattern of rasterisation is included in
The target position of tight spacing on sheet material, when observing on cross section, laser is sintered soot and simultaneously in sheet material
The first main surface on form recess, wherein the recess be zigzag so that at least some recesses have generally it is flat
Bottom surface and at least some corresponding adjacent crowns have the top surface of generally platform, and the top surface passes through into steep angle
The side wall and bottom surface of degree deviate.
19. the method being sintered as claimed in claim 18, wherein the pattern includes mobile to be generally the shape of polygon
Laser beam, wherein the vertex of polygonal shape is sphering.
20. the method being sintered as claimed in claim 18, wherein the recess is small recess, and the depth of each recess is extremely
Few 25nm and it is no more than 1 μm, the depth is relative to the higher person in the adjacent local crown on the either side of respective notches
Measurement, wherein each recess has the width for being at least 5 μm between adjacent local crown, and the length of each recess is extremely
It is 500 μm few.
Applications Claiming Priority (3)
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US201662376701P | 2016-08-18 | 2016-08-18 | |
US62/376,701 | 2016-08-18 | ||
PCT/US2017/047282 WO2018035286A1 (en) | 2016-08-18 | 2017-08-17 | Laser system and method forming a high purity fused silica glass sheet with micro-crenellations |
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CN109661379A true CN109661379A (en) | 2019-04-19 |
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WO (1) | WO2018035286A1 (en) |
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