METHOD FOR MANUFACTURING LARGE CERAMIC CO-FIRED ARTICLES
20200231509 ยท 2020-07-23
Assignee
Inventors
- Samuel H. Ahrendes (San Jose, CA, US)
- Gary D. Harland (Camas, WA, US)
- Chengtsin Lee (Union City, CA, US)
- Edward Tomasek (Costa Mesa, CA, US)
- George York (Citrus Height, CA, US)
Cpc classification
C04B2235/604
CHEMISTRY; METALLURGY
C04B2237/706
CHEMISTRY; METALLURGY
C04B37/021
CHEMISTRY; METALLURGY
C04B2235/95
CHEMISTRY; METALLURGY
C04B2237/704
CHEMISTRY; METALLURGY
C04B2235/5436
CHEMISTRY; METALLURGY
C04B2237/62
CHEMISTRY; METALLURGY
C04B2235/6028
CHEMISTRY; METALLURGY
B32B18/00
PERFORMING OPERATIONS; TRANSPORTING
C04B2235/3217
CHEMISTRY; METALLURGY
C04B2235/602
CHEMISTRY; METALLURGY
C04B2237/68
CHEMISTRY; METALLURGY
H05B3/283
ELECTRICITY
International classification
B32B18/00
PERFORMING OPERATIONS; TRANSPORTING
H01L21/67
ELECTRICITY
Abstract
A method of forming one or more high temperature co-fired ceramic articles, comprising the steps of:
a) forming a plurality of green compacts, by a process comprising dry pressing a powder comprising ceramic and organic binder to form a green compact;
b) disposing a conductor or conductor precursor to at least one surface of at least one of the plurality of green compacts to form at least one patterned green compact;
c) assembling the at least one patterned green compact with one or more of the plurality of green compacts or patterned green compacts or both to form a laminated assembly;
d) isostatically pressing the laminated assembly to form a pressed laminated assembly;
e) firing the pressed laminated assembly at a temperature sufficient to sinter the ceramic layers together.
Claims
1. A method of forming one or more high temperature co-fired ceramic electrostatic chucks, suitable for hot ion implantation, having an orthogonal dimension Z less than the X and Y dimensions, comprising: a) forming one or more green compacts comprising an inorganic component of 90 to 99.99% alumina, by a process comprising dry pressing a powder comprising ceramic and organic binder to form each of the one or more green compacts; b) disposing a conductor or conductor precursor to at least one surface layer of at least one of the one or more green compacts to form at least one heater patterned green compact and an electrode chuck patterned green compact; c) assembling an insulating green tape cast layer, which functions as a dielectric layer, to the electrostatic chuck electrode patterned green compact to form a laminated assembly; d) isostatically pressing the laminated assembly to form a pressed laminated assembly; e) firing the pressed laminated assembly at a temperature sufficient to sinter the alumina of the one or more green compacts and the insulating green tape cast layer together and to mould around the deposited conductor or conductor precursor to form a monolithic ceramic body with one or more electrically conductive electrodes embedded therein which function as electrical heating elements capable of thermal cycling between room temperature and 600 C.; wherein step (e) further comprises: i. supporting the pressed laminated assembly on an insulating_setter having at least one substantially flat surface; ii. mounting an insulating weight having at least one substantially flat surface on the pressed laminated assembly such that the pressed laminated assembly lies between the substantially flat surface of the insulating setter and the insulating weight.
2. The method as claimed in claim 1, wherein the at least one surface of the setter and/or weight is/are machined substantially flat.
3. The method as claimed in claim 1, wherein step (b) comprises applying a metallization layer to at least one surface of at least one of the one or more of the green compacts to form the at least one patterned green compact.
4. The method as claimed in claim 1, wherein the one or more green compacts comprise at least two green compacts, where step (c) further comprises positioning one or more shapes formed from a fugitive material between the at least two green compacts, whether either or both is patterned or not; and subsequent to step (d or e), the fugitive material is removed to leave hollow channels within the one or more high temperature co-fired ceramic articles.
5. The method as claimed in claim 1, wherein the one or more high temperature co-fired ceramic articles have an orthogonal dimension Z less than 10% of the longer of the X and Y dimension.
6. The method as claimed in claim 1, wherein the one or more high temperature co-fired ceramic articles have an orthogonal dimension Z less than 10% of the shorter of the X and Y dimension.
7. The method as claim in claim 1, wherein the dielectric layer is less than half the thickness of an adjacent dry pressed green compact, such that the dry pressed green compact suppresses the lack of uniformity of the skrinkage of the tape cast material.
8. A method of forming one or more high temperature co-fired ceramic electrostatic chucks having an orthogonal dimension Z less than the X and Y dimensions, comprising: a) forming one or more green compacts comprising an inorganic component of 90 to 99.99% alumina, by a process comprising dry pressing a powder comprising ceramic and organic binder to form each of the one or more green compacts; b) disposing a conductor or conductor precursor to at least one surface layer of at least one of the one or more green compacts to form at least one electrode chuck patterned green compact; c) assembling an insulating green tape cast layer, which functions as a dielectric layer, to the electrostatic chuck electrode patterned green compact to form a laminated assembly; d) isostatically pressing the laminated assembly to form a pressed laminated assembly; e) firing the pressed laminated assembly at a temperature sufficient to sinter the alumina of the one or more green compacts and the insulating green tape cast layer together and to mould around the deposited conductor or conductor precursor to form a monolithic ceramic body with one or more electrically conductive electrodes embedded therein, said tape cast layer being less than half the thickness of an adjacent dry pressed green compact, such that the dry pressed green compact suppresses the lack of uniformity of the skrinkage of the dielectric layer; wherein step (e) further comprises: i. supporting the pressed laminated assembly on an insulating_setter having at least one substantially flat surface; ii. mounting an insulating weight having at least one substantially flat surface on the pressed laminated assembly such that the pressed laminated assembly lies between the substantially flat surface of the insulating setter and the insulating weight.
9. The method as claimed in claim 8, wherein the tape cast layer is less than a quarter the thickness of an adjacent dry pressed green compact.
10. The method as claimed in claim 8, wherein the tape cast layer is less than a tenth the thickness of an adjacent dry pressed green compact.
11. The method as claimed in claim 8, wherein the electrostatic chuck comprises two dry pressed green compacts and one tape cast layer.
12. The method as claimed in claim 11, wherein a heater pattern lies between the two dry pressed green compacts and the electrostatic chuck pattern lies between the dry pressed green compact and the tape cast layer.
13. The method as claimed in claim 8, wherein the density of the one or more green compact after isostatic pressing is about 3.9 g/cc.
14. A method of forming one or more high temperature co-fired ceramic electrostatic chuck having an orthogonal dimension Z less than the X and Y dimensions comprising: a) forming one or more green compacts, by a process comprising dry pressing a powder comprising a ceramic and organic binder to form a green compact comprising an inorganic component of 90 to 99.99% alumina, titania, ZrO.sub.2, Y.sub.2O.sub.3, AlN, Si.sub.3N.sub.4, SiC, or combinations thereof; b) disposing a conductor or conductor precursor to at least one surface of at least one of the one or more green compacts to form at least one patterned green compact; c) assembling an insulating green material to the at least one patterned green compact to form a laminated assembly, wherein the insulating green material comprises an inorganic component of 90 to 99.99% alumina; d) isostatically pressing the laminated assembly to form a pressed laminated assembly; e) firing the pressed laminated assembly at a temperature sufficient to sinter the alumina of the one or more green compacts and the insulating green material together to form a monolithic ceramic body with one or more electrically conductive electrodes embedded therein.
15. A method according to claim 14, wherein the conductor or conductor precursor is selected from the group consisting of platinum, palladium, tungsten, molybdenum, niobium, tantalum and alloys thereof.
16. A method according to claim 14, wherein the conductor or conductor precursor comprises molybdenum.
17. A method according to claim 14, wherein the electrostatic chuck comprises a heater able to operate the electrostatic chuck up to 600 C.
18 The method as claimed in claim 14, wherein the density of the one or more green compact after isostatic pressing is about 3.9 g/cc.
19. A method according to claim 14, wherein the insulating green material is formed by dry pressing.
20. A method according to claim 14, wherein the step c) takes place in a wet hydrogen furnace.
Description
[0040] Further details and features of the invention will be apparent from the attached claims and following description made with reference to the accompany drawings in which.
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DETAILED DESCRIPTION
[0057] It is known that the roll compaction process for tape formation starts with spray drying of ceramic powder with organic binder, followed by feeding the ceramic powder into a roller to produce thin tapes. The pressing of powder between two rollers results in tape with non-uniform shrinkage in the XY direction. The present invention addresses these issues by using dry pressing method to produce thin sheets. Examples of a dry pressing technique include but are not limited to uniaxial pressing, die pressing, isopressing or a combination thereof. To maintain flexibility and lamination properties of the thin sheets and for the purpose of illustration of one example of the present invention, ceramic powders with organic additives similar to those commonly used in the roll compaction tape formation process are used as the raw material for the dry pressing tape.
[0058] Depending on the die size of dry presses, green sheets of large diameter (e.g. up to 1 m or more), thickness in the range from 1 mm up to 50 mm can be produced (as can sheets of thickness less than 1 mm). Such dry pressed sheet has good flexibility and is capable of receiving metallization paint that is screen printed or otherwise applied (e.g. ink jet printing, spray coating, spin coating, dip coating, numerically controlled dispensing) to produce large and thick HTCC devices.
[0059] Similar to standard tape processing, mechanical punch, waterjet, laser or other means can be used to shape layers and produce via holes in the green sheets.
[0060] After applying metallization paint, isostatic pressing is used to assemble multiple layers of green tapes and/or dry pressed green sheets. Typical pressures are up to about 103 MPa (15 k psi) but higher pressure may be used as required. Isostatic pressing not only produces good lamination between tapes but also ensures a uniform shrinkage of the multilayer tape structure during firing.
[0061] To demonstrate the feasibility of the current invention, a batch of 99.5% alumina powder was mixed with other inorganics, binder, plasticizer, dispersant and water to form a slurry, and subsequently spray dried to form a powder comprising the inorganics, binder, plasticizer, and dispersant.
[0062] The composition of the inorganic components of the spray dried powder is listed in Table 1. The alumina powder used was A152 SG from Almatis, Inc, which, form their data sheet, has an average particle size of 1.2 m and surface area of 4.3 m.sup.2/g.
TABLE-US-00001 TABLE 1 Magnesium Al.sub.2O.sub.3 carbonate EPK Kaolin Wt percent 99.2% 0.5% 0.3%
[0063] The binder can be any suitable material that provides adequate adhesion between the inorganic components after dry pressing to give an adherent yet flexible sheet. Typical binders include, for example, acrylic latexes, PVA, alkyd resins, polyethylene glycol, poly(methyl methacrylate), polyvinyl butyral, polyethyl oxazoline, polyacrylates, polyvinyl pyrolidone, cellulose, polyethylene, paraffin, and many more.
[0064] The plasticizer can be any suitable material that assists plastic deformation of the material. This is useful both during the dry pressing stage, and during the isostatic pressing (lamination) stage. Suitable materials include, for example, glycols, polyethylene glycols, mineral oil, phthalates, esters, benzyl butyl phthalate, polymers similar to the binder used but of lower molecular weight, and many more.
[0065] The dispersant is useful in ensuring that the slurry is well dispersed prior to spray drying so that the spray dried powder has good homogeneity. Typical dispersants include, for example, ammonium polyacrylate, ammonium citrate, fatty acids, corn oil, fish oil, amines, polyesters, polyamines, pH control substances (for example HCl or NH.sub.4OH), and many more.
[0066] Choice of binder, plasticizer (if any), and dispersant (if any) depends in part on their mutual compatibility achieving desired properties in a green compact and their behavior in a slurry, if spray drying is the route used to form the powder.
[0067] Typically, the inorganic components comprise over 50% by weight of the slurry, for example about 68%. Typical slurry formulations might be:
TABLE-US-00002 TABLE 2 Wt % in slurry Material Formulation 1 Formulation 2 Inorganics 68.2% 68.2% Water 24.0% 28.4% Dispersant 1.1% 0.9% Acrylic binder 0% 1.5% PVA binder 5.5% 0% Plasticiser 1.2% 0.9% (polyethylene glycol)
[0068] After spray drying, a portion of the spray dry powder was used to generate roll compaction tape. The remaining spray dry powder from the same batch was used to generate dry pressed sheets. The properties of a laminated body formed from roll compacted tape and dry pressed sheet is listed in Table 3.
TABLE-US-00003 TABLE 3 Roll compaction tape Dry pressed sheet Shrinkage factor* of 1.14 1.17 1.17 1.17 tape in the XY direction after about 103 MPa (15 kpsi) isostatic pressing and 1600 C. sintering Density# of tape/sheet after 3.9 g/cc 3.9 g/cc isostatic pressing and sintering *Shrinkage factor = XY dimensions of green part divided by same dimension of sintered part #Measured by water replacement (Archimedes).
[0069] From the above data, it is clear that the dry pressed sheets has more uniform shrinkage than that of the roll compaction tape. Both approaches have achieved nearly full density of the sintered alumina body, but the superior uniformity of shrinkage of the dry pressed sheet means that features may be positioned precisely in the body formed from dry pressed sheet. While it is not required that the green ceramic starting layer be tape as typically used in HTCC (High Temperature Co-Fired Ceramic) processing, typical tape processing can be used for this invention.
[0070] The improved HTCC processing method can be used to not only produce large size wafer processing apparatus for use in a ESC but also can be used to produce a multiplayer heater. The following examples are used to demonstrate the versatility of the improved HTCC processing method:
EXAMPLE 1
[0071] A multilayer heater is produced using the improved HTCC method as a demonstration of feasibility on a small scale.
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[0073] The process shown uses the spray dried 99.5% pure alumina powder mentioned previously. It should be noted that the present invention is not restricted to 99.5% alumina and can be used for other ceramics, [e.g. alumina of different purity (for example 90-99.9%), ZrO2, Y.sub.2O.sub.3, AlN, Si.sub.3N.sub.4, SiC, or indeed any ceramic].
[0074] At step 2, the spray dry powder is pressed (or uniaxially pressed) in a 2 die to produce thin sheets of about 1.5 mm thickness from the spray dried powder. The dry pressed green sheets is then cut in the green state to the desired shape (Step 4), e.g. by laser or water jet cutting.
[0075] Following cutting of the green sheets, the shaped dry pressed green sheets are metallized to deposit a metallization layer or metallic precursor on its surface (Step 6). In the particular embodiment, metallization involves screen printing, but other metallization techniques are permissible in the present invention, e.g. ink jet printing, spraying etc. The use of a metallic precursor enables techniques such as ink printing to be used. Although a Mo (molybdenum) based metallization is used in the particular embodiment, other conductive material can be used such as conductive material selected from the group consisting of platinum, palladium, gold, tungsten, molybdenum, niobium, tantalum and alloys of any of the foregoing. After screen printing the dry pressed green sheets with Mo based metallization (Wesgo 538 paint) measures approximately 25 m in thickness (which after firing leads to a metal thickness of 20 m; four layers of the dry pressed green sheets are laminated together using a rubber die in an isostatic press at a pressure of 103 MPa (15 kpsi) (Step 8). Also shown in
[0076] After lamination, the pressed assembly of green sheets is sintered or co-fired in an Astro furnace using wet H.sub.2 gas to 1600 C. at a pressure of 1 atm (Step 12) to form a monolithic insulating ceramic body having one or more electrical conductors embedded therein.
[0077] After sintering, the four layer 20 heater is ground to the final shape (Step 16). Prior to machining the fired assembly, the assembly can optionally be tested at this stage (Step 14) to test the performance of the co-fired assembly as a heater 20. Electric contacts are made with the metallization layers, e.g. by means of vias, and an electric current is passed through the metallization layers to test the heating performance of the heater. In the particular embodiment, electrodes 24 (See
[0078] A kovar hard plate 26 is brazed on top of the heater using a lower temperature braze alloy (Incusil).
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EXAMPLE 2
[0080] The objective of the example is to demonstrate the new HTCC processing method can be used to produce large sized wafer processing apparatus such as heater and electrostatic chuck (ESC) combination or electrostatic chuck (ESC). The goal is to ensure the 300 mm heater is capable of thermal cycling between room temperature and 600 C. with good temperature uniformity.
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[0082] The spray dried powder is dry pressed using a 2500 ton dry press (uniaxial press) with an 81 cm diameter die to generate green sheets of 81 cm diameter with thickness in the range of about 2.5 mm to 6 mm (Step 34). In the particular embodiment where the ESC is used in combination with a heater, the combination may be based on assembling three dry pressed sheets formed from two outside dry pressed sheets and a centre dry pressed sheet. The two outside pressed sheets has a thickness of about 5 mm or 6 mm and the centre dry pressed sheet has a thickness of about 2.5 mm. Further detail of the arrangement of the dry pressed sheets is discussed below with reference to
[0083] The dry pressed green sheet is then water jet cut to a 30 cm diameter with alignment holes (some or all of which may serve as lift pin holes in the finished heater) (Step 36) as demonstrated in
[0084]
[0085] The laminated and isostatically pressed part 60 is placed over Mo and alumina setters 66 and sintered in an Astro hydrogen furnace in a wet hydrogen atmosphere to 1600 C. at a pressure of 1 atm (
[0086] The firing regime (Step 42) can comprises a slow binder burn out phase, in which the temperature is raised at a rate of 1 C. per minute up to a temperature sufficient to burn off the binder (typically, 275 to 400 C.) followed by ramping up at a rate of about 3 C./minute up to the sintering temperature (typically 1500 C. to 1600 C.) in hydrogen. After 2-3 hours at temperature, the temperature is ramped down (e.g. at a rate of 3 C./minute) to a temperature low enough to remove the sintered parts.
[0087] Carrying out binder burn off and sintering in the same furnace provides a one step process, as well as the ability to process multiple samples simultaneously in the furnace are advantageous over the complexity of hot pressing. However, alternative processes can be adopted, for example conducting the binder burn off and sintering steps in separate furnaces. In some cases, it is advantageous to treat the laminated and isostatically pressed part 60 in separate oven/furnaces because the conditions for debinding and/or binder burn out can be different to firing. For example, for debinding/binder burn off it is important that any volatiles generated during binder burnout do not introduce any defects or flaws in the pressed part, and as a result the set up for binder burn out is different to firing. For binder burn out it is necessary to ensure that there is adequate exposure of the entire exterior surface area of the dry pressed sheets for binder removal, since the volatiles generated during binder burnout would need to escape and be purged. However, since there is limited exposure to the underside of the dry pressed part as it is resting on the setter 66, a spacer is used to elevate the dry pressed sheet above the setter. This ensures that there is sufficient air flow to the underside of the laminated part to promote binder removal (pyrolysis of the binder). In the particular embodiment shown in
[0088] In the firing process the wax filling the holes melts away leaving access points or vias for electrical connection to the metallization layer(s) and/or location points for locating the electrostatic chuck on a pedestal in substrate processing.
[0089] After densification, the fired parts 68 are hard ground (typically by Blanchard grinding) to the final dimension (Step 44) with an optional gas groove and various lift-pin holes (through holes for wafer ejection).
[0090] Subsequently, mounting pin and electrical feedthroughs 70 are brazed onto the heater/ESC plate using a high temperature braze (
[0091] Co-firing the laminated assembly generates a monolithic insulating ceramic body comprising one or more layers of electrical conductors provided by the metallization layers embedded therein.
[0092] In the embodiment, where the ESC is located on top of a heater as shown in
Additional Operations
Void Formation
[0093] Providing wax (or otherwise) filled holes as described above permits the optional formation of channels running across the thickness of the article. For example, where cooling is required to the electrostatic chuck, one or more channels or voids can be incorporated into the insulating ceramic body. To produce hollow channels 84 within the thickness of an article made by this method, it is possible to press shapes formed from a fugitive material between the layers of dry pressed sheet and subsequently burn off or otherwise remove the fugitive material.
[0094] Materials that can be used include wax, plastics, paper or flexible graphite,(e.g. Grafoil)
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[0096] Such hollow channels can be used for a variety of purposes including: to provide gas supply or extraction channels; for filling with materials [e.g. metals to provide large conductors]; or even providing channels for the flow of a heat transfer fluid for cooling purposes.
Dielectric Layer
[0097] To generate an electrostatic force across the surface of the electrostatic chuck, the thickness of the ceramic layer forming the dielectric layer has to be sufficiently flat and thin to within acceptable tolerances so as to cooperate with the underlying electrodes.
[0098] While dry pressing is an excellent way of forming sheets, even of thickness as low as, for example, 0.25 mm, the thinner the sheet the more problematic is its formation.
[0099] When it is desired to provide just a thin surface layer [e.g. less than 1 mm, less than 0.5 mm, less than 0.25 mm, or less than 0.1 mm] for the dielectric layer then laminating a layer of tape cast material over a thicker dry pressed sheet can optionally be used with advantage. This is particularly so when the layer of tape cast is less than, for example, half the thickness of the dry pressed sheet or less than a quarter the thickness of the dry pressed sheet, or less than a tenth the thickness of the dry pressed sheet. In such an arrangement the uniformity of shrinkage of the dry pressed sheet can dominate, or even suppress the lack of uniformity of shrinkage of the tape cast material.
[0100] Such a process can be used to form an electrostatic chuck on top of the heater described in Example 2. For example (as indicated in
[0104] In the case where the dry pressed green sheet has a thickness of approximately 6 mm, after firing the fired dry pressed sheet shrinks to a thickness, d.sub.1, of approximately 5 mm. For the 2.5 mm thickness green dry pressed sheet, after firing the dry pressed sheet shrinks to a thickness, d.sub.2 of approximately 2 mm. Likewise, after firing the thickness of the green tape cast layer shrinks to a smaller thickness, d.sub.3. In this process, the tape cast layer functions as the dielectric layer and is an outermost layer of the assembly, but for other applications the tape cast layer may lie within the assembly, e.g. between two dry pressed sheets.
[0105] Although the tape cast layer is advantageous in producing thin layers which is ideal as a dielectric layer since the tape cast layer is fabricated through a different process to a dry pressing process (e.g. uniaxial die pressing), differential shrinkage can result between the tape cast layer and the dry pressed layers during de-binding and/or firing. This could be due to a combination of the different binder content between a dry pressed sheet and a tape cast layer which is inherent in their fabrication process as well to the different internal stresses as a result of their particular processing techniques. As a result, during de-binding or firing of the green sheets such differential shrinkage can cause the tape cast layer to de-laminate from the dry pressed sheets or even crack.
[0106] To mitigate this problem, in an alternative embodiment of the present invention, the dielectric layer can be fabricated from an additional dry pressed green sheet. Instead of laminating the metallization layer with a tape cast layer 95 described with reference to
[0110] After firing using the flat firing process discussed above, the laminated assembly forms a monolithic-metal composite part (see
[0111]
[0112] The number of metalized dry pressed green sheets in the assembly depends upon whether the assembly is purely used as an ESC or a combination of an ESC together with a heater. For example, in the case where the ECS is used to retain the semiconductor wafer for cleaning purposes or etching etc., no heater may be required and the metallization layer 76 that represents the heater can simply be absent, i.e. the ESC comprises an electrostatic electrode pattern 78 sandwiched between two dry pressed green sheets. Where the ESC is used in combination with a heater, then the number of metallization layers increases; one metallization layer provides the electrodes 78 that cooperate with the dielectric layer 86 to generate an electrostatic field for electrostatically clamping a substrate (semiconductor wafer) in use and a further metallization layer 76 is applied on another dry pressed green sheet to permit electrical heating. Different combinations of dry pressed green sheets and metallization layers representing the electrostatic pattern and/or heater pattern and/or voids is/are permissible in the present invention, each combination depends on their particular application, e.g. electrostatic clamping purposes or a combination of electrostatic clamping and heating or cooling.
[0113] The present invention has the advantages of providing an HTCC process suited for the manufacture of large objects, and does not require either hot pressing or the handling of delicate wire meshes [as does U.S. Pat. No. 6,225,606].
[0114] Further features, modifications and uses of the invention will be apparent to the skilled person desiring to make objects by high temperature co-firing, and are encompassed within the scope of this invention.