US20160031188A1 - High Strength Carbon Fiber Composite Wafers For Microfabrication - Google Patents
High Strength Carbon Fiber Composite Wafers For Microfabrication Download PDFInfo
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- US20160031188A1 US20160031188A1 US14/874,235 US201514874235A US2016031188A1 US 20160031188 A1 US20160031188 A1 US 20160031188A1 US 201514874235 A US201514874235 A US 201514874235A US 2016031188 A1 US2016031188 A1 US 2016031188A1
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- B32B27/00—Layered products comprising a layer of synthetic resin
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- B32B27/34—Layered products comprising a layer of synthetic resin comprising polyamides
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- B32B3/26—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer
- B32B3/266—Layered products comprising a layer with external or internal discontinuities or unevennesses, or a layer of non-planar form; Layered products having particular features of form characterised by a particular shape of the outline of the cross-section of a continuous layer; characterised by a layer with cavities or internal voids ; characterised by an apertured layer characterised by an apertured layer, the apertures going through the whole thickness of the layer, e.g. expanded metal, perforated layer, slit layer regular cells B32B3/12
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- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
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- B32B37/18—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with all layers existing as coherent layers before laminating involving the assembly of discrete sheets or panels only
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- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21K—TECHNIQUES FOR HANDLING PARTICLES OR IONISING RADIATION NOT OTHERWISE PROVIDED FOR; IRRADIATION DEVICES; GAMMA RAY OR X-RAY MICROSCOPES
- G21K1/00—Arrangements for handling particles or ionising radiation, e.g. focusing or moderating
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- H01J5/00—Details relating to vessels or to leading-in conductors common to two or more basic types of discharge tubes or lamps
- H01J5/02—Vessels; Containers; Shields associated therewith; Vacuum locks
- H01J5/18—Windows permeable to X-rays, gamma-rays, or particles
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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- Y10T428/24124—Fibers
Definitions
- the present application is related generally to high strength microstructures, such as for example x-ray window support structures.
- Carbon fiber composite (CFC) wafers can be used in applications where high strength is desired. Barriers to the development of carbon fiber based structures, especially structures with micrometer-sized features, include difficulties in machining or patterning, and high surface roughness of cured composites.
- the present invention is directed to a method of making a carbon fiber composite (CFC) wafer that satisfies the needs for high strength and low surface roughness.
- the method comprises pressing a stack of at least one sheet of CFC between pressure plates with a porous breather layer disposed between at least one side of the stack and at least one of the pressure plates; then heating the stack to a temperature of at least 50° C. to cure the stack into a CFC wafer.
- the present invention is directed to a carbon fiber composite (CFC) wafer that satisfies the needs for high strength and low surface roughness.
- the CFC wafer comprises at least one sheet of CFC including carbon fibers embedded in a matrix.
- the wafer can have a thickness of between 10-500 micrometers.
- the wafer can have a root mean square surface roughness Rq, on at least one side, of less than 300 nm in an area of 100 micrometers by 100 micrometers and less than 500 nm along a line of 2 millimeter length.
- the wafer can have a yield strength at fracture of greater than 0.5 gigapascals, wherein yield strength is defined as the force, in a direction parallel with a plane of the wafer, per unit area, to cause the wafer to fracture.
- the wafer can have a strain at fracture of more than 0.01, wherein strain is defined as the change in length caused by a force in a direction parallel with a plane of the wafer divided by original length.
- the present invention is directed to an x-ray window including a high strength support structure.
- the x-ray window can comprise a support frame defining a perimeter and an aperture with a plurality of ribs extending across the aperture of the support frame and carried by the support frame. Openings exist between the plurality of ribs.
- the support frame and the plurality of ribs comprise a support structure.
- a film can be disposed over, can be carried by, and can span the plurality of ribs and can be disposed over and can span the openings.
- the film can be configured to pass x-ray radiation therethrough.
- the support structure can comprise a carbon fiber composite material (CFC).
- the CFC material can comprise carbon fibers embedded in a matrix.
- a thickness of the support structure can be between 10-500 micrometers.
- a root mean square surface roughness Rq of the support structure on a side facing the film can be less than 500 nm along a line of 2 millimeter length.
- FIG. 1 is a schematic top view of a carbon fiber composite wafer, in accordance with an embodiment of the present invention
- FIGS. 2-3 are schematic cross-sectional side views of a carbon fiber composite wafer, in accordance with an embodiment of the present invention.
- FIG. 4 is a schematic cross-sectional side view of portion of a carbon fiber composite wafer, showing measurement of root mean square surface roughness Rq, in accordance with an embodiment of the present invention
- FIG. 5 is a side view of a carbon fiber, in accordance with an embodiment of the present invention.
- FIG. 6 is a schematic cross-sectional side view of wafer including multiple carbon fiber composite sheets abutting a polyimide sheet, in accordance with an embodiment of the present invention
- FIG. 7 illustrates a first curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention
- FIG. 8 illustrates use of o-rings and a vacuum during the first curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention
- FIG. 9 illustrates a second curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention.
- FIG. 10 is a schematic top view of an x-ray window support structure, in accordance with an embodiment of the present invention.
- FIG. 11 is a schematic cross-sectional side view of an x-ray window, in accordance with an embodiment of the present invention.
- FIG. 12 is a schematic cross-sectional side view of an x-ray detector, including an x-ray window, in accordance with an embodiment of the present invention.
- carbon fiber or “carbon fibers” means solid, substantially cylindrically shaped structures having a mass fraction of at least 85% carbon, a length of at least 5 micrometers and a diameter of at least 1 micrometer.
- the term “directionally aligned,” in referring to alignment of carbon fibers with support structure members (such as ribs for example), means that the carbon fibers are substantially aligned with a longitudinal axis of the support structure members and does not require the carbon fibers to be exactly aligned with a longitudinal axis of the support structure members.
- porous means readily permeable to gas.
- CFC carbon fiber composite
- the matrix can comprise a material that provides sufficient strength and is compatible with the use of the wafer. For example, if the wafer will be used to fabricate an x-ray window support structure, considerations for matrix material may include a low atomic number elements and low outgassing.
- the matrix can comprise a material selected from the group consisting of polyimide, bismaleimide, epoxy, or combinations thereof.
- the matrix can comprise a material selected from the group consisting of amorphous carbon, hydrogenated amorphous carbon, nanocrystalline carbon, microcrystalline carbon, hydrogenated nanocrystalline carbon, hydrogenated microcrystalline carbon, or combinations thereof.
- the matrix can comprise a ceramic material selected from the group consisting of silicon nitride, boron nitride, boron carbide, aluminum nitride, or combinations thereof.
- the carbon fibers 12 can be directionally aligned in a single direction Al, directionally aligned in multiple directions, or disposed in random directions in the matrix.
- Three CFC sheets 21 a - c are shown in FIGS. 2-3 . There may be more or less CFC sheets 21 than 3 , depending on the desired application.
- the wafer 20 can have a thickness Th w of between 10-500 micrometers in one aspect, between 20 and 350 micrometers in another aspect, less than or equal to 20 micrometers in another aspect, or greater than or equal to 350 micrometers in another aspect.
- CFC wafers per the present invention can have high yield strength.
- a yield strength at fracture can be greater than 0.1 gigapascals (GPa) in one aspect, greater than 0.5 GPa in another aspect, greater than 2 GPa in another aspect, between 2 GPa and 3.6 GPa in another aspect, or between 0.5 GPa and 6 GPa in another aspect.
- Yield strength can be defined as a force F in a direction parallel with a plane 33 or 34 of a side 32 a or 32 b of the wafer, per unit area, to cause the wafer to fracture. If fibers are directionally aligned, the force F can be aligned parallel with the fibers.
- CFC wafers per the present invention can have high strain.
- a strain at fracture can be greater than 0.01 in one aspect, greater than 0.03 in another aspect, greater than 0.05 in another aspect, or between 0.01 and 0.080 in another aspect.
- Strain can be defined as the change in length L caused by a force F in a direction parallel with a plane 33 or 34 of the wafer divided by original length L. If fibers are directionally aligned, the force F can be aligned parallel with the fibers.
- the wafer can have two faces or sides 32 a - b and an edge 31 .
- the sides 32 a - b can have a substantially larger surface area than the edge 31 .
- the sides 32 a - b can be substantially parallel with each other.
- One side 32 a can be disposed along, or parallel with, a single plane 33 ; and the other side 32 b can be disposed along, or parallel with, a different single plane 34 .
- At least one side 32 a and/or 32 b of the wafer can be smooth, i.e. can have a low surface roughness.
- a low surface roughness can be beneficial for improving adhesion to other materials, such as to an x-ray window film for example.
- the measurement z i can be made along a surface of the wafer by an atomic force microscope.
- the measurement of z i on a portion of the wafer 40 is shown in FIG. 4 .
- a distance from a plane 43 , substantially parallel with the wafer, or substantially parallel with the sides 32 a and 32 b of the wafer, can differ by small amounts.
- the root mean square surface roughness Rq of one or both sides of the wafers of the present invention can be less than 300 nm in one aspect, or between 30 nm and 300 nm in another aspect, in an area of 100 micrometers by 100 micrometers.
- the root mean square surface roughness Rq of one or both sides of the wafers of the present invention can be less than 500 nm in one aspect, or between 50 nm and 500 nm in another aspect, along a line of 2 millimeter length.
- the root mean square surface roughness Rq of one or both sides of the wafers of the present invention can be less than 200 nanometers in one aspect, or between 20 nm and 200 nm in another aspect, in an area of 100 micrometers by 100 micrometers.
- FIG. 5 Shown in FIG. 5 is a side view of a carbon fiber 12 , in accordance with an embodiment of the present invention. At least 50% of the carbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in one aspect. At least 90% of the carbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in another aspect. Substantially all of the carbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in another aspect.
- a polyimide sheet 61 can be cured together with and can abut the sheet(s) 21 of carbon fiber composite.
- the polyimide sheet can have a thickness Th p , after curing, of between 0.1-100 micrometers.
- each carbon fiber composite sheet 21 a - c in the stack can have a thickness Th a-c of between 20 to 350 micrometers (20 ⁇ m ⁇ Th a ⁇ 350 ⁇ m, 20 ⁇ m ⁇ Th b ⁇ 350 ⁇ m, and 20 ⁇ m ⁇ Th c ⁇ 350 ⁇ m) in one aspect, less than or equal to 20 micrometers in another aspect, or greater than or equal to 350 micrometers in another aspect. There may be more or less than the three carbon fiber composite sheets 21 a - c. These thicknesses are sheet 21 thicknesses after curing.
- FIG. 7 illustrates a first curing process 70 for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention.
- the method can comprise providing a stack 71 of at least one sheet of CFC 21 a - c, the stack having a first surface 32 a and a second surface 32 b; pressing P the stack between a first pressure plate 76 a and a second pressure plate 76 b with a porous breather layer 72 disposed between the first surface 32 a of the stack and the first pressure plate 76 a; and curing by heating the stack 71 to a temperature of at least 50° C. (defining a first curing process).
- the amount of pressure to be used can depend on the matrix of the carbon composite. Pressure in the range of 50-200 psi has been successfully used. Pressure may be in the range of 25-500 psi.
- a solid, polished layer 73 can be disposed between the second surface 32 b of the stack 71 and the second pressure plate 76 b during the first curing process.
- the polished layer 73 can help create a very smooth surface on the second surface 32 b of the stack 71 .
- the polished layer 73 can be a highly polished sheet of stainless steel, a silicon wafer, or a glass plate.
- a fluorine release layer can be used to avoid the stack sticking 71 to the polished layer 73 .
- a fluorinated alkane monolayer can be deposited on silicon wafers to facilitate release by placing in a vacuum desiccator overnight with 5 mL of Trichloro(1H,1H,2H,2H-perfluorooctyl)silane in a glass vial.
- the polished layer 73 can have a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack. Thus, it is not necessary for the polished layer 73 to have a polished surface on both sides.
- a polyimide sheet 61 can be cured together with and can abut the CFC sheet(s) 21 .
- the polyimide sheet 61 can be disposed between the second surface 32 b of the stack 71 and the second pressure plate 76 b.
- the polyimide sheet 61 can be disposed between the second surface 32 b of the stack 71 and the polished layer 73 (if a polished layer is used).
- a polyimide sheet 61 can be disposed on both surfaces 32 a and 32 b of the stack 71 .
- the polyimide sheet(s) 61 can be useful for improving the surface of the final wafer and/or for improving adhesion of the stack 71 to other materials.
- the porous layer 72 can allow gas, emitted by the stack, to escape from the press.
- a multi-layer porous breather layer 72 can be used.
- the porous breather layer 72 can comprise a porous polymer layer 72 b facing the stack 71 and a nylon mesh 72 a facing the first pressure plate 76 a.
- a vacuum can aid in removal of the gas.
- a vacuum pump 75 can be attached by tubing 74 to the press and can draw a vacuum, such as less than 50 torr, between the pressure plates. The vacuum can be maintained through substantially all of the curing process, or through only part of the curing process, such as at least 50% of the curing process.
- the layers (stack of CFC, porous breather layer 72 , optional polished layer 73 , and optional polyimide layer 61 ) 81 can be in a central portion of the pressure plates 76 a - b.
- An o-ring 82 can surround the layers 81 .
- the o-ring 82 can be disposed at least partly in a channel 83 of at least one of the pressure plates 76 a and/or 76 b.
- the vacuum tube 74 can extend into the central portion of the press, between the layers 81 and the o-ring 82 .
- FIG. 9 illustrates a second curing process 90 for manufacture of a carbon fiber composite wafer in accordance with a method of the present invention.
- pressure P can be released from the stack and the porous layer 72 can be removed from the stack.
- a polished layer 73 a and 73 b can be disposed on each side of the stack. Note that if there was a polyimide sheet 61 in the first curing process, this polyimide sheet 61 can remain for the second curing process 90 .
- the polished layers 73 a and 73 b can have a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack.
- the stack 71 (and optional polyimide sheet 61 if one is used) can be pressed between the polished layers by the first and second pressure plates 76 a - b.
- the stack 71 (and optional polyimide layer 61 ) can be cured by heating the stack to a temperature of at least 50° C.
- a benefit of use of the second curing process 90 is that the gas can be removed during the first curing process 70 , then polished layers 73 a and 73 b can be disposed on both sides 32 a and 32 b of the stack 71 , with the result that both sides of the wafer can be highly polished.
- both sides of the wafer can have a root mean square surface roughness Rq as specified above.
- the support structure 100 can comprise a support frame 101 defining a perimeter 104 and an aperture 105 .
- a plurality of ribs 102 can extend across the aperture 105 of the support frame 101 and can be carried by the support frame 101 , with openings 103 between the ribs 102 .
- the support frame 101 and the plurality of ribs 102 can comprise a support structure 100 .
- the support structure 100 can comprise a carbon fiber composite (CFC) material.
- the CFC material can comprise carbon fibers embedded in a matrix.
- Carbon fibers 12 in the composite can be substantially aligned with a direction Al of the ribs, with at least one direction of the ribs if the ribs extend in multiple directions, or with all directions of all ribs if the ribs extend in multiple directions.
- Carbon fibers in a carbon fiber composite can be graphitic, and thus can be highly resistant to chemical etching.
- Alternative methods have been found for etching or cutting micro-sized structures in CFC wafers in the present invention.
- the support structure 100 may be made by cutting a CFC wafer to form ribs 102 and openings 103 .
- the CFC wafer may be cut by laser milling or laser ablation.
- a high power laser can use short pulses of laser to ablate the material to form the openings 103 by ultrafast laser ablation.
- a femtosecond laser may be used.
- a nanosecond pulsed YAG laser may be used. Ablating wafer material in short pulses of high power laser can be used in order to avoid overheating the CFC material.
- a non-pulsing laser can be used and the wafer can be cooled by other methods, such as conductive or convective heat removal.
- the wafer can be cooled by water flow or air across the wafer.
- the above mentioned cooling methods can also be used with laser pulses, such as a femtosecond laser, if additional cooling is needed.
- the support structure 100 can have a thickness Th s of between 10-500 micrometers. Tops of the ribs 102 and support frame 101 can terminate substantially in a single plane 116 .
- a film 114 can be disposed over, can be carried by, and can span the plurality of ribs 102 and can be disposed over and can span the openings 103 .
- the film 114 can be configured to pass radiation therethrough, such as by being made of a material and thickness that will allow x-ray radiation to pass through with minimal attenuation of x-rays and/or minimal contamination of the x-ray signal.
- a polyimide layer 61 can be cured abutting the CFC stack 71 .
- the polyimide layer 61 can be cut into polyimide ribs 111 and a polyimide support frame 112 , with openings 103 between the ribs 111 , along with the CFC stack 71 .
- the polyimide ribs 111 and the polyimide support frame 112 can be part of the support structure 100 .
- the polyimide ribs 111 and the polyimide support frame 112 can be disposed between the CFC stack 71 and the film 114 .
- a surface of the support structure 100 facing the film can have low surface roughness.
- This surface can be CFC 71 or can be polyimide 61 .
- This surface can have a root mean square surface roughness Rq of less than 300 nm in one aspect, or between 30 nm and 300 nm in another aspect, in an area of 100 micrometers by 100 micrometers.
- This surface can have a root mean square surface roughness Rq of less than 500 nm in one aspect, or between 50 nm and 500 nm in another aspect, along a line of 2 millimeter length.
- This surface can have a root mean square surface roughness Rq of less than 200 nanometers in one aspect, or between 20 nm and 200 nm in another aspect, in an area of 100 micrometers by 100 micrometers.
- the ribs 102 can have a strain at fracture of greater than 0.01 in one aspect, greater than 0.03 in another aspect, greater than 0.05 in another aspect, or between 0.01 and 0.080 in another aspect. Strain can be defined as a change in length caused by a force in a direction parallel with the ribs divided by original length. If fibers are directionally aligned, the force F can be aligned parallel with the fibers.
- the wafers described herein can also be micropatterned by laser ablation and/or water jet to form other structures, such as a flexure mechanical mechanism, a mesoscale mechanical mechanism, a microscale mechanical mechanism, and/or elements in a microelectromechanical system (MEMS).
- MEMS microelectromechanical system
- an x-ray window 125 including a support structure 100 and a film 114 , can be hermetically sealed to a housing 122 .
- the housing can contain an x-ray detector 123 .
- the x-ray detector can be configured to receive x-rays 124 transmitted through the window, and to output a signal based on x-ray energy.
Abstract
A method of making a high strength carbon fiber composite (CFC) wafer with low surface roughness comprising at least one sheet of CFC including carbon fibers embedded in a matrix. A stack of at least one sheet of CFC is provided with the stack having a first surface and a second surface. The stack is pressed between first and second pressure plates with a porous breather layer disposed between the first surface of the stack and the first pressure plate. The stack is cured by heating the stack to a temperature of at least 50° C.
Description
- This is a divisional of U.S. patent application Ser. No. 13/667,273, filed Nov. 2, 2012; which claims priority to U.S. Provisional Patent Application Ser. No. 61/689,392, filed on Jun. 6, 2012; and which is a continuation-in-part of U.S. patent application Ser. No. 13/453,066, filed on Apr. 23, 2012, which claims priority to U.S. Provisional Patent Application Nos. 61/486,547, filed on May 16, 2011; 61/495,616, filed on Jun. 10, 2011; and 61/511,793, filed on Jul. 26, 2011; all of which are hereby incorporated herein by reference in their entirety.
- The present application is related generally to high strength microstructures, such as for example x-ray window support structures.
- Carbon fiber composite (CFC) wafers can be used in applications where high strength is desired. Barriers to the development of carbon fiber based structures, especially structures with micrometer-sized features, include difficulties in machining or patterning, and high surface roughness of cured composites. A root mean square surface roughness Rq of typical CFC wafers can be greater than 1 micrometer. Root mean square surface roughness Rq can be defined by the following equation: Rq=√{square root over (Σzi 2)}. In this equation, z represents a height of the surface at different measured locations i.
- It has been recognized that it would be advantageous to have a carbon fiber composite wafer having high strength and low surface roughness.
- In one embodiment, the present invention is directed to a method of making a carbon fiber composite (CFC) wafer that satisfies the needs for high strength and low surface roughness. The method comprises pressing a stack of at least one sheet of CFC between pressure plates with a porous breather layer disposed between at least one side of the stack and at least one of the pressure plates; then heating the stack to a temperature of at least 50° C. to cure the stack into a CFC wafer.
- In another embodiment, the present invention is directed to a carbon fiber composite (CFC) wafer that satisfies the needs for high strength and low surface roughness. The CFC wafer comprises at least one sheet of CFC including carbon fibers embedded in a matrix. The wafer can have a thickness of between 10-500 micrometers. The wafer can have a root mean square surface roughness Rq, on at least one side, of less than 300 nm in an area of 100 micrometers by 100 micrometers and less than 500 nm along a line of 2 millimeter length. The wafer can have a yield strength at fracture of greater than 0.5 gigapascals, wherein yield strength is defined as the force, in a direction parallel with a plane of the wafer, per unit area, to cause the wafer to fracture. The wafer can have a strain at fracture of more than 0.01, wherein strain is defined as the change in length caused by a force in a direction parallel with a plane of the wafer divided by original length.
- In another embodiment, the present invention is directed to an x-ray window including a high strength support structure. The x-ray window can comprise a support frame defining a perimeter and an aperture with a plurality of ribs extending across the aperture of the support frame and carried by the support frame. Openings exist between the plurality of ribs. The support frame and the plurality of ribs comprise a support structure. A film can be disposed over, can be carried by, and can span the plurality of ribs and can be disposed over and can span the openings. The film can be configured to pass x-ray radiation therethrough. The support structure can comprise a carbon fiber composite material (CFC). The CFC material can comprise carbon fibers embedded in a matrix. A thickness of the support structure can be between 10-500 micrometers. A root mean square surface roughness Rq of the support structure on a side facing the film can be less than 500 nm along a line of 2 millimeter length.
-
FIG. 1 is a schematic top view of a carbon fiber composite wafer, in accordance with an embodiment of the present invention; -
FIGS. 2-3 are schematic cross-sectional side views of a carbon fiber composite wafer, in accordance with an embodiment of the present invention; -
FIG. 4 is a schematic cross-sectional side view of portion of a carbon fiber composite wafer, showing measurement of root mean square surface roughness Rq, in accordance with an embodiment of the present invention; -
FIG. 5 is a side view of a carbon fiber, in accordance with an embodiment of the present invention; -
FIG. 6 is a schematic cross-sectional side view of wafer including multiple carbon fiber composite sheets abutting a polyimide sheet, in accordance with an embodiment of the present invention; -
FIG. 7 illustrates a first curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention; -
FIG. 8 illustrates use of o-rings and a vacuum during the first curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention; -
FIG. 9 illustrates a second curing process for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention; -
FIG. 10 is a schematic top view of an x-ray window support structure, in accordance with an embodiment of the present invention; -
FIG. 11 is a schematic cross-sectional side view of an x-ray window, in accordance with an embodiment of the present invention; -
FIG. 12 is a schematic cross-sectional side view of an x-ray detector, including an x-ray window, in accordance with an embodiment of the present invention. - As used herein, the term “carbon fiber” or “carbon fibers” means solid, substantially cylindrically shaped structures having a mass fraction of at least 85% carbon, a length of at least 5 micrometers and a diameter of at least 1 micrometer.
- As used herein, the term “directionally aligned,” in referring to alignment of carbon fibers with support structure members (such as ribs for example), means that the carbon fibers are substantially aligned with a longitudinal axis of the support structure members and does not require the carbon fibers to be exactly aligned with a longitudinal axis of the support structure members.
- As used herein, the term “porous” means readily permeable to gas.
- Illustrated in
FIGS. 1-3 are carbon fiber composite (CFC) wafers 10 and 20 comprising at least oneCFC sheet 21 includingcarbon fibers 12 embedded in amatrix 11. The matrix can comprise a material that provides sufficient strength and is compatible with the use of the wafer. For example, if the wafer will be used to fabricate an x-ray window support structure, considerations for matrix material may include a low atomic number elements and low outgassing. The matrix can comprise a material selected from the group consisting of polyimide, bismaleimide, epoxy, or combinations thereof. The matrix can comprise a material selected from the group consisting of amorphous carbon, hydrogenated amorphous carbon, nanocrystalline carbon, microcrystalline carbon, hydrogenated nanocrystalline carbon, hydrogenated microcrystalline carbon, or combinations thereof. The matrix can comprise a ceramic material selected from the group consisting of silicon nitride, boron nitride, boron carbide, aluminum nitride, or combinations thereof. - The
carbon fibers 12 can be directionally aligned in a single direction Al, directionally aligned in multiple directions, or disposed in random directions in the matrix. ThreeCFC sheets 21 a-c are shown inFIGS. 2-3 . There may be more orless CFC sheets 21 than 3, depending on the desired application. Thewafer 20 can have a thickness Thw of between 10-500 micrometers in one aspect, between 20 and 350 micrometers in another aspect, less than or equal to 20 micrometers in another aspect, or greater than or equal to 350 micrometers in another aspect. - CFC wafers per the present invention can have high yield strength. A yield strength at fracture can be greater than 0.1 gigapascals (GPa) in one aspect, greater than 0.5 GPa in another aspect, greater than 2 GPa in another aspect, between 2 GPa and 3.6 GPa in another aspect, or between 0.5 GPa and 6 GPa in another aspect. Yield strength can be defined as a force F in a direction parallel with a
plane side - CFC wafers per the present invention can have high strain. A strain at fracture can be greater than 0.01 in one aspect, greater than 0.03 in another aspect, greater than 0.05 in another aspect, or between 0.01 and 0.080 in another aspect. Strain can be defined as the change in length L caused by a force F in a direction parallel with a
plane - The wafer can have two faces or sides 32 a-b and an
edge 31. The sides 32 a-b can have a substantially larger surface area than theedge 31. The sides 32 a-b can be substantially parallel with each other. Oneside 32 a can be disposed along, or parallel with, asingle plane 33; and theother side 32 b can be disposed along, or parallel with, a differentsingle plane 34. - At least one
side 32 a and/or 32 b of the wafer can be smooth, i.e. can have a low surface roughness. A low surface roughness can be beneficial for improving adhesion to other materials, such as to an x-ray window film for example. One measurement of surface roughness is root mean square surface roughness Rq calculated by the equation Rq=√{square root over (Σzi 2)}. The measurement zi can be made along a surface of the wafer by an atomic force microscope. The measurement of zi on a portion of thewafer 40 is shown inFIG. 4 . A distance from aplane 43, substantially parallel with the wafer, or substantially parallel with thesides - Shown in
FIG. 5 is a side view of acarbon fiber 12, in accordance with an embodiment of the present invention. At least 50% of thecarbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in one aspect. At least 90% of thecarbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in another aspect. Substantially all of thecarbon fibers 12 in a wafer can have a diameter D of between 2 and 10 micrometers in another aspect. - As shown on
wafer 60 inFIG. 6 , apolyimide sheet 61 can be cured together with and can abut the sheet(s) 21 of carbon fiber composite. The polyimide sheet can have a thickness Thp, after curing, of between 0.1-100 micrometers. - Also shown on
wafer 60 inFIG. 6 are carbon fiber composite sheet thicknesses Tha-c. Each carbonfiber composite sheet 21 a-c in the stack can have a thickness Tha-c of between 20 to 350 micrometers (20 μm<Tha<350 μm, 20 μm<Thb<350 μm, and 20 μm<Thc<350 μm) in one aspect, less than or equal to 20 micrometers in another aspect, or greater than or equal to 350 micrometers in another aspect. There may be more or less than the three carbonfiber composite sheets 21 a-c. These thicknesses aresheet 21 thicknesses after curing. -
FIG. 7 illustrates afirst curing process 70 for manufacture of a carbon fiber composite wafer, in accordance with a method of the present invention. The method can comprise providing astack 71 of at least one sheet ofCFC 21 a-c, the stack having afirst surface 32 a and asecond surface 32 b; pressing P the stack between afirst pressure plate 76 a and asecond pressure plate 76 b with aporous breather layer 72 disposed between thefirst surface 32 a of the stack and thefirst pressure plate 76 a; and curing by heating thestack 71 to a temperature of at least 50° C. (defining a first curing process). The amount of pressure to be used can depend on the matrix of the carbon composite. Pressure in the range of 50-200 psi has been successfully used. Pressure may be in the range of 25-500 psi. - A solid,
polished layer 73 can be disposed between thesecond surface 32 b of thestack 71 and thesecond pressure plate 76 b during the first curing process. Thepolished layer 73 can help create a very smooth surface on thesecond surface 32 b of thestack 71. Thepolished layer 73 can be a highly polished sheet of stainless steel, a silicon wafer, or a glass plate. A fluorine release layer can be used to avoid the stack sticking 71 to thepolished layer 73. For example, a fluorinated alkane monolayer can be deposited on silicon wafers to facilitate release by placing in a vacuum desiccator overnight with 5 mL of Trichloro(1H,1H,2H,2H-perfluorooctyl)silane in a glass vial. Thepolished layer 73 can have a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack. Thus, it is not necessary for thepolished layer 73 to have a polished surface on both sides. - A
polyimide sheet 61 can be cured together with and can abut the CFC sheet(s) 21. Thepolyimide sheet 61 can be disposed between thesecond surface 32 b of thestack 71 and thesecond pressure plate 76 b. Thepolyimide sheet 61 can be disposed between thesecond surface 32 b of thestack 71 and the polished layer 73 (if a polished layer is used). Alternatively, apolyimide sheet 61 can be disposed on bothsurfaces stack 71. The polyimide sheet(s) 61 can be useful for improving the surface of the final wafer and/or for improving adhesion of thestack 71 to other materials. - The
porous layer 72 can allow gas, emitted by the stack, to escape from the press. A multi-layerporous breather layer 72 can be used. For example, theporous breather layer 72 can comprise aporous polymer layer 72 b facing thestack 71 and anylon mesh 72 a facing thefirst pressure plate 76 a. A vacuum can aid in removal of the gas. Avacuum pump 75 can be attached bytubing 74 to the press and can draw a vacuum, such as less than 50 torr, between the pressure plates. The vacuum can be maintained through substantially all of the curing process, or through only part of the curing process, such as at least 50% of the curing process. - Shown in
FIG. 8 are more details of the press and vacuum. The layers (stack of CFC,porous breather layer 72, optionalpolished layer 73, and optional polyimide layer 61) 81 can be in a central portion of the pressure plates 76 a-b. An o-ring 82 can surround thelayers 81. The o-ring 82 can be disposed at least partly in achannel 83 of at least one of thepressure plates 76 a and/or 76 b. Thevacuum tube 74 can extend into the central portion of the press, between thelayers 81 and the o-ring 82. -
FIG. 9 illustrates asecond curing process 90 for manufacture of a carbon fiber composite wafer in accordance with a method of the present invention. After completion of thefirst curing process 70, pressure P can be released from the stack and theporous layer 72 can be removed from the stack. Apolished layer polyimide sheet 61 in the first curing process, thispolyimide sheet 61 can remain for thesecond curing process 90. The polished layers 73 a and 73 b can have a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack. The stack 71 (andoptional polyimide sheet 61 if one is used) can be pressed between the polished layers by the first and second pressure plates 76 a-b. The stack 71 (and optional polyimide layer 61) can be cured by heating the stack to a temperature of at least 50° C. - A benefit of use of the
second curing process 90 is that the gas can be removed during thefirst curing process 70, then polished layers 73 a and 73 b can be disposed on bothsides stack 71, with the result that both sides of the wafer can be highly polished. Thus, both sides of the wafer can have a root mean square surface roughness Rq as specified above. - Shown in
FIG. 10 is asupport structure 100 for an x-ray window. Thesupport structure 100 can comprise asupport frame 101 defining aperimeter 104 and anaperture 105. A plurality ofribs 102 can extend across theaperture 105 of thesupport frame 101 and can be carried by thesupport frame 101, withopenings 103 between theribs 102. Thesupport frame 101 and the plurality ofribs 102 can comprise asupport structure 100. Thesupport structure 100 can comprise a carbon fiber composite (CFC) material. The CFC material can comprise carbon fibers embedded in a matrix.Carbon fibers 12 in the composite can be substantially aligned with a direction Al of the ribs, with at least one direction of the ribs if the ribs extend in multiple directions, or with all directions of all ribs if the ribs extend in multiple directions. - Carbon fibers in a carbon fiber composite can be graphitic, and thus can be highly resistant to chemical etching. Alternative methods have been found for etching or cutting micro-sized structures in CFC wafers in the present invention. The
support structure 100 may be made by cutting a CFC wafer to formribs 102 andopenings 103. The CFC wafer may be cut by laser milling or laser ablation. A high power laser can use short pulses of laser to ablate the material to form theopenings 103 by ultrafast laser ablation. A femtosecond laser may be used. A nanosecond pulsed YAG laser may be used. Ablating wafer material in short pulses of high power laser can be used in order to avoid overheating the CFC material. Alternatively, a non-pulsing laser can be used and the wafer can be cooled by other methods, such as conductive or convective heat removal. The wafer can be cooled by water flow or air across the wafer. The above mentioned cooling methods can also be used with laser pulses, such as a femtosecond laser, if additional cooling is needed. - As shown in
FIG. 11 , thesupport structure 100 can have a thickness Ths of between 10-500 micrometers. Tops of theribs 102 andsupport frame 101 can terminate substantially in asingle plane 116. Afilm 114 can be disposed over, can be carried by, and can span the plurality ofribs 102 and can be disposed over and can span theopenings 103. Thefilm 114 can be configured to pass radiation therethrough, such as by being made of a material and thickness that will allow x-ray radiation to pass through with minimal attenuation of x-rays and/or minimal contamination of the x-ray signal. - As described above regarding
FIGS. 6-9 , apolyimide layer 61 can be cured abutting theCFC stack 71. Thepolyimide layer 61 can be cut intopolyimide ribs 111 and apolyimide support frame 112, withopenings 103 between theribs 111, along with theCFC stack 71. Thepolyimide ribs 111 and thepolyimide support frame 112 can be part of thesupport structure 100. Thepolyimide ribs 111 and thepolyimide support frame 112 can be disposed between theCFC stack 71 and thefilm 114. - A surface of the
support structure 100 facing the film can have low surface roughness. This surface can beCFC 71 or can be polyimide 61. This surface can have a root mean square surface roughness Rq of less than 300 nm in one aspect, or between 30 nm and 300 nm in another aspect, in an area of 100 micrometers by 100 micrometers. This surface can have a root mean square surface roughness Rq of less than 500 nm in one aspect, or between 50 nm and 500 nm in another aspect, along a line of 2 millimeter length. This surface can have a root mean square surface roughness Rq of less than 200 nanometers in one aspect, or between 20 nm and 200 nm in another aspect, in an area of 100 micrometers by 100 micrometers. - The
ribs 102 can have a strain at fracture of greater than 0.01 in one aspect, greater than 0.03 in another aspect, greater than 0.05 in another aspect, or between 0.01 and 0.080 in another aspect. Strain can be defined as a change in length caused by a force in a direction parallel with the ribs divided by original length. If fibers are directionally aligned, the force F can be aligned parallel with the fibers. - The wafers described herein can also be micropatterned by laser ablation and/or water jet to form other structures, such as a flexure mechanical mechanism, a mesoscale mechanical mechanism, a microscale mechanical mechanism, and/or elements in a microelectromechanical system (MEMS).
- As shown in
FIG. 12 , anx-ray window 125, including asupport structure 100 and afilm 114, can be hermetically sealed to ahousing 122. The housing can contain anx-ray detector 123. The x-ray detector can be configured to receivex-rays 124 transmitted through the window, and to output a signal based on x-ray energy.
Claims (20)
1. A method of making a wafer, the method comprising:
a. providing a stack of at least one sheet of carbon fiber composite (CFC) including carbon fibers embedded in a matrix, the stack having a first surface and a second surface;
b. pressing the stack between first and second pressure plates with a porous breather layer disposed between the first surface of the stack and the first pressure plate; and
c. curing by heating the stack to a temperature of at least 50° C., defining a first curing process.
2. The method of claim 1 , further comprising disposing a solid, polished layer between the second surface of the stack and the second pressure plate during the first curing process with the polished layer having a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack.
3. The method of claim 1 , further comprising:
a. releasing pressure from the stack;
b. removing the porous layer from the stack;
c. disposing a polished layer on each side of the stack, the polished layers having a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers, on a side facing the stack; and
d. pressing the stack and polished layers between first and second pressure plates;
e. curing by heating the stack to a temperature of at least 50° C., defining a second curing process.
4. The method of claim 1 , wherein the porous breather layer comprises a porous polymer layer facing the stack and a nylon mesh facing the first pressure plate.
5. The method of claim 1 , wherein providing the stack includes a sheet of polyimide disposed adjacent to the second surface of the stack.
6. The method of claim 1 , wherein curing by heating the stack includes creating a vacuum of less than 50 torr between the pressure plates, and maintaining the vacuum through at least 50% of the curing process.
7. The method of claim 1 , wherein each sheet in the stack has a thickness of between 20 to 350 micrometers.
8. The method of claim 1 , further comprising micropatterning the wafer by laser ablation, water jet, or combinations thereof to form an x-ray window support structure comprising:
a. a support frame defining a perimeter and an aperture;
b. a plurality of ribs extending across the aperture of the support frame and carried by the support frame;
c. openings between the plurality of ribs; and
d. the support frame and the plurality of ribs comprising a support structure.
9. The method of claim 1 , wherein at least 90% of the carbon fibers have a diameter of between 2 and 10 micrometers.
10. The method of claim 1 , wherein the matrix comprises a material selected from the group consisting of polyimide, bismaleimide, epoxy, or combinations thereof.
11. The method of claim 1 , wherein the matrix comprises a material selected from the group consisting of amorphous carbon, hydrogenated amorphous carbon, nanocrystalline carbon, microcrystalline carbon, hydrogenated nanocrystalline carbon, hydrogenated microcrystalline carbon, or combinations thereof.
12. The method of claim 1 , wherein the matrix comprises a ceramic material selected from the group consisting of silicon nitride, boron nitride, boron carbide, aluminum nitride, or combinations thereof.
13. The method of claim 1 , further comprising a polyimide sheet cured together with and abutting the at least one sheet of carbon fiber composite.
14. The method of claim 13 , wherein the polyimide sheet has a thickness of between 0.1-100 micrometers.
15. The method of claim 1 , wherein the matrix comprises polyimide.
16. The method of claim 1 , wherein the matrix comprises bismaleimide.
17. A wafer formed by the method of claim 1 , wherein the wafer comprises:
a. a wafer thickness of between 10-500 micrometers;
b. at least one side of the wafer having a root mean square surface roughness Rq of less than 300 nm in an area of 100 micrometers by 100 micrometers and less than 500 nm along a line of 2 millimeter length;
c. a yield strength at fracture of greater than 0.5 gigapascals (GPa), wherein yield strength is defined as a force, in a direction parallel with a plane of a side of the wafer, per unit area, to cause the wafer to fracture; and
d. a strain at fracture of more than 0.01, wherein strain is defined as the change in length caused by a force in a direction parallel with a plane of the wafer divided by original length.
18. The wafer of claim 17 , wherein the yield strength is between 2 GPa and 3.6 GPa.
19. The wafer of claim 17 , wherein the root mean square surface roughness is less than 200 nanometers in an area of 100 micrometers by 100 micrometers.
20. The wafer of claim 17 micropatterned by laser ablation, water jet, or combinations thereof to form an x-ray window support structure comprising:
a. a support frame defining a perimeter and an aperture;
b. a plurality of ribs extending across the aperture of the support frame and carried by the support frame;
c. openings between the plurality of ribs; and
d. the support frame and the plurality of ribs comprising a support structure.
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US9174412B2 (en) | 2011-05-16 | 2015-11-03 | Brigham Young University | High strength carbon fiber composite wafers for microfabrication |
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