The present invention relates to diagnostic device for the characterization of electromagnetic material properties and a method of making and using same.
The need for high performance materials has been increasing by leaps and bounds due to the explosion new technologies such hypersonic flight. Unfortunately, the ability to test such materials at the extreme conditions that are required by their end use has as remained not been adequately explored due to the speed of the developments in the technology area. In particular, the ability to assess the permittivity, permeability, and the loss tangent of materials of high performance materials at extreme conditions has not been addressed. Applicants recognized that the source of the problem was found in the design and composition of test fixtures as well as the manner in which the test conditions were generated. Unlike current diagnostic devices, the disclosed diagnostic device is suitable for the characterization of electromagnetic material properties such as permittivity, permeability, and the loss tangent of materials over a broad temperature and pressure range. The disclosed diagnostic device employs inductive heating coupled with a novel waveguide system, inert gas pressurization or vacuum capability, a fluid cooling system and an advanced sensor and analysis system to achieve the aforementioned benefits.
The present invention relates to diagnostic device for the characterization of electromagnetic material properties and a method of making and using same. Unlike current diagnostic devices, the disclosed diagnostic device comprises a novel waveguide system and is suitable for the characterization of electromagnetic material properties such as permittivity, permeability, and the loss tangent of materials over a broad temperature and pressure range.
Additional objects, advantages, and novel features of the invention will be set forth in part in the description which follows, and in part will become apparent to those skilled in the art upon examination of the following or may be learned by practice of the invention. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the present invention and, together with a general description of the invention given above, and the detailed description of the embodiments given below, serve to explain the principles of the present invention.
Unless specifically stated otherwise, as used herein, the terms “a”, “an” and “the” mean “at least one”.
As used herein, the terms “include”, “includes” and “including” are meant to be non-limiting.
As used herein, the words “about,” “approximately,” or the like, when accompanying a numerical value, are to be construed as indicating a deviation as would be appreciated by one of ordinary skill in the art to operate satisfactorily for an intended purpose.
As used herein, the words “and/or” means, when referring to embodiments (for example an embodiment having elements A and/or B) that the embodiment may have element A alone, element B alone, or elements A and B taken together.
Unless otherwise noted, all component or composition levels are in reference to the active portion of that component or composition, and are exclusive of impurities, for example, residual solvents or by-products, which may be present in commercially available sources of such components or compositions.
All percentages and ratios are calculated by weight unless otherwise indicated. All percentages and ratios are calculated based on the total composition unless otherwise indicated.
It should be understood that every maximum numerical limitation given throughout this specification includes every lower numerical limitation, as if such lower numerical limitations were expressly written herein. Every minimum numerical limitation given throughout this specification will include every higher numerical limitation, as if such higher numerical limitations were expressly written herein. Every numerical range given throughout this specification will include every narrower numerical range that falls within such broader numerical range, as if such narrower numerical ranges were all expressly written herein.
Applicants disclose a waveguide system.
For purposes of this specification, headings are not considered paragraphs and thus this paragraph is paragraph sixty-four of the present specification. The individual number of each paragraph above and below this paragraph can be determined by reference to this paragraph's number. In this paragraph sixty-four, Applicants disclose a waveguide system comprising:
Applicants disclose the waveguide system of paragraph sixty-four wherein;
Applicants disclose the waveguide system of paragraphs sixty-four through sixty-five wherein at least one of said removable connections comprises a plurality of threaded fasteners.
Applicants disclose the waveguide system of paragraphs sixty-four through sixty-six wherein each removable connection comprises a plurality of threaded fasteners.
Applicants disclose the waveguide system of paragraphs sixty-four through sixty-seven wherein at least one waveguide adapter comprises a slit.
Applicants disclose the waveguide system of paragraphs sixty-four through sixty-eight comprising one or more heaters, preferably said waveguide system comprises an induction heater, a radiative heater and/or a furnace heater, preferably each of said heaters is independently a radiative heater and/or an induction heater, more preferably each of said heaters is an induction heater.
Applicants disclose the waveguide system of paragraphs sixty-four through sixty-nine wherein each of said threaded fasteners are independently selected from the group consisting of bolts and/or studs, preferably each of said threaded fasteners is a bolt.
Applicants disclose the waveguide system of paragraphs sixty-four through seventy wherein said first and second vacuum or pressure cooling components comprise a plurality of vacuum fittings, a vacuum through hole to the waveguide through hole, a plurality of water cooling connections and a liquid cooling channel, preferably said first and second vacuum or pressure cooling components comprise at least 8 fittings or from to 8 to 14 vacuum fittings, a vacuum through hole to the waveguide through hole, at least 22 water cooling connections or from 22 to 30 water cooling connections and a liquid cooling channel.
Applicants disclose the waveguide system of paragraphs sixty-four through seventy-one wherein said high temperature waveguide comprises a refractory metal and an oxidation protective coating; preferably said refractory metal is selected from the group consisting of molybdenum and molybdenum alloys, more preferably said refractory metal is a molybdenum alloy, most preferably said refractory metal is Titanium-Zirconium-Molybdenum alloy, and preferably said oxidation protective coating is a Silicon/Boron/Carbon oxidation protective coating, preferably said Silicon/Boron/Carbon oxidation protective coating has an atomic ratio of Silicon/Boron/Carbon that is 1:10:2. A suitable Silicon/Boron/Carbon oxidation protective coating has an atomic ratio of Silicon/Boron/Carbon that is 1:10:2 is SIBOR®. Plansee SE located at Metallwerk-Plansee-Str. Reutte, Austria 716600 can apply SIBOR® coatings to objects.
Applicants disclose the waveguide system of paragraphs sixty-four through seventy-two wherein each waveguide component's waveguide through hole is axial with respect to each waveguide component.
Applicants disclose the waveguide system of paragraphs sixty-four through seventy-three wherein each waveguide component's waveguide through hole is rectangular, square or circular.
Applicants disclose the waveguide system of sixty-four through seventy-four wherein said oxidation protective coating is coated with a ceramic that comprises zirconium oxide.
Applicants disclose a diagnostic device, said device comprising a waveguide system of paragraphs sixty-four through seventy-five.
Applicants disclose the diagnostic device of paragraph seventy-five said diagnostic device comprising a vector network analyzer and a computer.
A hermetic low-loss impedance matched window is required for narrow band characterization. For example, when considering X-Band frequency, this window typically consists of quartz fixed in a small waveguide section as seen in sheet 10 of the drawings. In addition to the window material, an iris implemented to impedance match the window at a particular frequency. With two impedance matched windows at the same frequency, a sample material can be characterized at a temperature of interest.
Before material characterization can begin, a transmission reflection & line (TRL) calibration must be performed on the vector network analyzer (VNA) at the temperature of interest. This is performed while the waveguide system is assembled. And example of the assembled system is shown on sheet 1 of the drawings.
Referring to
If the coefficient of thermal expansion of the sample is lower than the waveguide when the sample fully fills the waveguide at room temperature, then an air gap will form between the heated waveguide section and sample when the waveguide heated section is heated. When air gaps are present, an air gap correction must be made, which is explained below. If the coefficient of thermal expansion of the sample is higher than the waveguide, then the sample must be smaller than the waveguide before being heated. For best results, the sample should completely fill the waveguide at the temperature of interest.
After the TRL calibration has taken place, the waveguide should be gradually brought down to room temperature if it was heated. One side should be disassembled, a sample placed directly in the center of the heated waveguide system, and then reassembled. After this is done, the waveguide heated section should be brought up to the temperature of interested and held there until the system reaches thermal equilibrium. After this, S parameters should be recorded using the TRL calibration of the temperature of interest. These S parameters are noted as S11c, S21c, S12c, S22c.
To extract the complex permittivity and complex permeability of the sample material at the temperature of interest, and at the matched frequency of the windows, the following operations must be performed.
First, the averaged
Here ω is the angular frequency of the matched frequency of the window, c is the speed of light in a vacuum, and
An example of calculating the average waveguide width is given below. This graphic assumes symmetry at the center of the waveguide heated section. The length from the ends of waveguide adapters up to the heated waveguide section would have a length of z1. From the ends of the heated waveguide section, held as close to room temperature as possible using the cooling sections, up to a uniformly heated region of the heated waveguide section, would have a length of z2. The uniformly heated section would have a length of z3. Then the total length of the assembled waveguide minus the coaxial waveguide adapters is given by
z=2z1+2z2+z3
And the average waveguide width is given by
a
=L
a(2z1/z)+(La+ΔLa/2)(2z2/z)+(La+ΔLa)(z3/z)
With the average propagation constant (
S
11
s
=S
11
c
e
j
(d+Δ)
S
21
s
=S
21
c
e
−j
Δ
S
12
s
=S
12
c
e
−j
Δ
S
22
s
=S
22
c
e
−j2
Δ
If the calibration plane is at port 1, then the following must be done.
S
11
s
=S
11
c
e
−j2
Δ
S
21
s
=S
21
c
e
−j
Δ
S
12
s
=S
12
c
e
−j
Δ
S
22
s
=S
22
c
e
j
(d+Δ)
From here, if no gaps exist between the sample and the heated waveguide, relative complex permittivity and complex permeability of the sample can be extracted with the following procedures.
V
1
=S
21
s
+S
11
s
V
2
=S
21
s
−S
11
s
X=(1−V1V2)/(V1−V2)
Γ=X±√{square root over (X2−1)}(Γ<1)
P=(V1−Γ)/(1−ΓV1)
βs=(2jπn−ln(P))/jLs n=0,1,2 . . .
Here the integer n is chosen to be the number of wavelengths within the sample. For example, if a sample is extremely thin, then n would be chosen to be 0 unless permittivity or permeability were significantly high.
The process is again repeated except V1 and V2 are defined from the de-embedded S12 and S22 taken from the VNA.
The extracted values of μr and εr are then averaged to give
μr=[μr(S22_S12)+μr(S22_S12)]/2
εr=[εr(S22_S12)+εr(S11_S21)]/2
So long as the sample isn't a multiple of a half-guided wavelength and the waveguide is completely filled, the results will be most accurate at the matched frequency of the windows. The results can be even more accurate for non-magnetic materials by assuming relative permeability μr(S11_S21) and μr(S22_S12) are equal to 1.
If air gaps exist between the sample and the waveguide, then an air gap correction must take place. It is important to note that large air gaps will introduce significant error into the measurement for samples with higher values of permittivity and permeability. The air gap must typically be less than 1% of the total height of the sample. The following procedures can be used to correct for air gaps from the previously extracted values of relative complex permittivity and complex permeability.
Δb=(Lb−Lbs)/Lb
μr′=(μ′r−Δb)/(1−Δb)
μr″=μr″/(1−Δb)
εr′=εr′(1−Δb)/(1−Δbεr′)
εr″=εr″(1−Δb)/(1−Δbεr″)2
μr=μr′+μr″
εr=εr′+εr″
Here εr′ and μr′ are the real portions of the extracted complex permittivity and permeability while εr′ and μr″ are the imaginary portions. Finally, complex permittivity and permeability are given by
ε=ε0εr
μr=μ0μr
To characterize isotropic materials over the bandwidth of the waveguide, a hermetic window section (sheet 10 of the drawings) which fully fills the waveguide cross section with a low loss material must be used. For example, an X-Band waveguide (8-12 GHz) could utilize a quartz window as it is a low loss material for that frequency range. Unlike the narrowband method, no iris should be present on this window.
To begin the characterization process. First, the complex permittivity and permeability of the window sections, the pressure/cooling sections, and the heated waveguide sections must be known. These parameters can be extracted using a simpler form of the narrowband method described above and a different TRL calibration method. A TLR calibration method is only required at room temperature for characterizing the window section and the pressure/cooling sections. This calibration is performed by using only the waveguide adapters. After the calibration is performed, S-parameters of the window section and pressure/cooling section are acquired by using only the waveguide adapters and the section of interest, one at a time.
Because the waveguide adapters are used directly on each section, no de-embedding is required and the S-parameters translate directly to the surface of the section being measured, given below.
S
11
s
=S
11
c
S
21
s
=S
21
c
S
12
s
=S
12
c
S
22
s
=S
22
c
Using these parameters, the complex permittivity and permeability of each section can be extracted using the methods described in narrowband characterization section. These components are likely to have a real relative permeability of 1 with no imaginary component. Furthermore, no air gap correction is needed.
After this is performed, the waveguide system needs to be assembled with no sample inside of it. The next step is to characterize the heated waveguide section's permittivity and permeability as a function of temperature. Referring to
Their corresponding relative complex permittivity (εr) and permeability are given as (μr)
The waveguide adapter has a propagation constant of.
Notice this is not an average waveguide propagation constant as there is no thermal expansion in this section. The left and rightmost waveguide sections also have the same propagation constant.
β(0)=β(1)=β(7)
Here β0 represent the propagation constant at a waveguide adapter to the left of the assembled system. β1 and β7 represent the propagation constants in the waveguide sections at the left and right ends of the assembled system.
In the window section, the cooling/pressure section, and the heated waveguide sections have propagation constants given by
β(i)=√{square root over (k02εr(i)μr(i)−kw2)} for i=2,3,4,5,6
Where εr2 and μr2 are the extracted relative complex permittivity and complex permeability of the window section, respectively. The same is true for εr6 and μr6. In the same manner εr3 and μr3 are the relative complex permittivity and complex permeability of the pressure/window section, respectively. The same is true for εr5 and μr5.
Finally, the heated waveguide section's values (εr(4) and μr(4)) over different temperatures will need to be found using a root-finding algorithm, such as the Newton-Raphson method. The purely real values of 1 is a good starting guess value for εr(4) and μr(4). This value will change and converge to a value as the root finding algorithm proceeds.
The next steps are to construct a matrix with these initial values to be used in a root finding algorithm. First, admittance numbers are constructed for each section and the waveguide adapter
A
(i)=β(i)/(k0η0) for i=0,1,2,3,4,5,6,7
Where the free space impedance η0 is given by
η0=√{square root over (μ0/ε0)}
ε0=8.8541878128×10−12
μ0=1.25663706212×10−6
The admittance matrix M is then constructed using phase information from the propagation constants
Ψi=β(i)Δz(i) for i=0,1,2,3,4,5,6,
The following constants are then generated.
C
0=β0−i cot(β1)Δz0A0
C
1
=i csc(β1)Δz0A0
C
2
=iA
1 csc(Ψ1)
C
3
=−i[A
1 cot(Ψ1)+A2 cot(Ψ2)]
C
4
=C
5
=iA
2 csc(Ψ2)
C
6
=−i[A
2 cot(Ψ2)+A3 cot(Ψ3)]
C
7
=C
8
=iA
3 csc(Ψ3)
C
9
=−i[A
3 cot(Ψ3)+A4 cot(Ψ4)]
C
10
=C
11
=iA
4 csc(Ψ4)
C
12
=−i[A
4 cot(Ψ4)+A5 cot(Ψ5)]
C
13
=C
14
=iA
5 csc(Ψ5)
C
15
=−i[A
5 cot(Ψ5)+A6 cot(Ψ6)]
C
16
=C
17
=iA
6 csc(Ψ6)
C
18
=−i[A
6 cot(Ψ6)+A7 cot(Ψ7)]
C
19
=iA
7 csc(Ψ7)
With these values the admittance matrix takes the form.
The admittance matrix is then inverted and multiplied by T to obtain theoretical S parameters.
The theoretical S-parameters are then compared to the measured S-parameters of the VNA, and the function (F1) needs to be minimized through iteration. This is done by changing the values of εr(4) and #r(4) through each iteration.
F1=(Re(S11_Theoretical−S11_Measured))2+(Im(S11_Theoretical−S11_Measured))2+(Re(S21_Theoretical−S21_Measured))2+(Im(S21_Theoretical−S21_Measured))2
The S22 and S12 parameters can also be compared by rearranging the M matrix as follows.
Using the same methods to obtain
F2=(Re(S22_Theoretical−S22_Measured))2+(Im(S22_Theoretical−S22_Measured))2(Re(S12_Theoretical−S12_Measured))+(Im(S12_Theoretical−S12_Measured))2
The value of εr(4) and μr(4) associated with F1 and the values of εr(4) and μr(4) associated with F2 can then be averaged.
εr(4)=(εr(4,F1)+εr(4,F2))/2
μr(4)=(μr(4,F1)+μr(4,F2))/2
From here the values of εr(4) and μr(4) at a particular temperature have been characterized and can now be used in a similar process to extract complex permittivity and complex permeability of a sample placed directly in the center of the heated waveguide.
Once again, an admittance matrix must be assembled which will be a 10 by 10 matrix as the sample placed directly in the center of heated waveguide section will divide it into a left side and a right side. Then the lengths will be given as:
The left (Δz(4)) and right (Δz(6)) heated waveguide section lengths will be equal if the sample is placed directly in the middle of the heated waveguide sections. Their lengths will be half of the total heated waveguide section length minus the sample length.
Each section's corresponding relative complex permittivity (εr) and permeability are given as (μr)
Notice the sections containing εr(2), εr(3), εr(4), εr(6), εr(7), εr(8) and μr(2), μr(3), μr(4), μr(6), μr(7), μr(8) were already previously characterized in prior steps. Again, the waveguide adapter has a propagation constant of
The left and rightmost waveguide sections also have the same propagation constant.
β(0)=β(1)=β(9)
And all other sections the propagation constant is given by
β(i)=√{square root over (k02εr(i)μr(i)−kw2)} for i=2,3,4,5,6,7,8
The sample section's values (εr(5) and μr(5)) over different temperatures will need to be guessed to be used in a root-finding algorithm. A value found using the narrowband method, at a particular temperature, is a good starting guess for these values.
The admittance matrix M is then constructed using phase information from the propagation constants
Ψi=β(i)Δz(i) for i=0,1,2,3,4,5,6,7,8,9
C
0=β0−i cot(β1)Δz0A0
C
1
=i csc(β1)Δz0A0
C
2
=iA
1 csc(Ψ1)
C
3
=−i[A
1 cot(Ψ1)+A2 cot(Ψ2)]
C
4
=C
5
=iA
2 csc(Ψ2)
C
6
=−i[A
2 cot(Ψ2)+A3 cot(Ψ3)]
C
7
=C
8
=iA
3 csc(Ψ3)
C
9
=−i[A
3 cot(Ψ3)+A4 cot(Ψ4)]
C
10
=C
11
=iA
4 csc(Ψ4)
C
12
=−i[A
4 cot(Ψ4)+A5 cot(Ψ5)]
C
13
=C
14
=iA
5 csc(Ψ5)
C
15
=−i[A
5 cot(Ψ5)+A6 cot(Ψ6)]
C
16
=C
17
=iA
6 csc(Ψ6)
C
18
=−i[A
6 cot(Ψ6)+A7 cot(Ψ7)]
C
19
=C
20
=iA
7 csc(Ψ7)
C
21
=−i[A
6 cot(Ψ7)+A7 cot(Ψ8)]
C
22
=C
23
=iA
7 csc(Ψ8)
C
24
=−i[A
6 cot(Ψ8)+A7 cot(Ψ9)]
C
25
=iA
7 csc(Ψ9)
Which can be used to find theoretical S-parameters using
And again
For
S
22_Theoretical
=P
[1,1]−1
S
12_Theoretical
=P
[10,1]
Then again, the theoretical S-parameters are then compared to the measured S-parameters of the VNA, and the function (F) needs to be minimized through iteration. This is done by changing the values of εr(6) and μr(6) through each iteration.
F1=(Re(S11_Theoretical−S11_Measured))2+(Im(S11_Theoretical−S11_Measured))2+(Re(S21_Theoretical−S21_Measured))2+(Im(S21_Theoretical−S21_Measured))2
F2=(Re(S22_Theoretical−S22_Measured))2+(Im(S22_Theoretical−S22_Measured))2+(Re(S12_Theoretical−S12_Measured))+(Im(S12_Theoretical−S12_Measured))2
The value of εr(6) and μr(6) associated with F1 and the values of εr(6) and μr(6) associated with F2 can then be averaged.
εr(4)=(εr(6,F1)+εr(6,F2))/2
μr(4)=(μr(6,F1)+μr(6,F2))/2
Finally, if an air gap is present, these values can then be used in the air gap correction method as outlined in the narrowband section.
The following examples illustrate particular properties and advantages of some of the embodiments of the present invention. Furthermore, these are examples of reduction to practice of the present invention and confirmation that the principles described in the present invention are therefore valid but should not be construed as in any way limiting the scope of the invention.
Example 1. The experimental apparatus consists of several components as seen in
Example 2. A brief overview of the characterization process at room temperature will be explained. First, a sample material is placed within a waveguide. Then an electromagnetic wave having a TE10 mode is sent through one end of the waveguide. The portion of the wave that passes through the sample is considered to have been transmitted through it. The other portions of the wave that are not transmitted can then either be reflected off the sample or be absorbed by the sample.
k
wg
=π/a, k
0=2πf/c
With these wavenumbers, the propagation constant (βwg) inside the empty waveguide is given by the equation below.
βwg=√{square root over (k02−(kwg)2)}
The S-parameters obtained by a network analyzer must then be de-embedded. This process is necessary because the S-parameters need to be moved from the end ports of the waveguide to the faces of the sample material. By knowing the propagation constant within the waveguide as well as the distances from the ports to the sample, the S-parameters can then be de-embedded (Benjamin Reid Crowgey, 2013). In the equations below j=√{square root over (−1)}.
S
11
′=S
11
e
2jβ
d
S
21
′=S
21
e
2jβ
(d
+d
)
S
22
′=S
22
e
2jβ
d
S
12
′=S
12
e
2jβ
(d
+d
)
After the S-parameters have been de-embedded, algebraic manipulation allows us to solve for the interfacial reflection coefficient (Γ) and the propagation factor (P).
We then arrive to the propagation constant within the sample material (βs). In the equation below n=1 if the sample size is kept under a quarter wavelength. This is experimentally achieved by using small lengths in the dimension of ds is measured
From here complex permittivity (εr) and permeability (μr) can be extracted at room temperature. Note that these values will be complex since the S-parameters are complex. Additionally, and average can be taken be switching S11′→S22′ and S21′→S12′ in the equations above.
The extracted values of complex εr and μr are only good so long as the sample material completely fills the waveguide. If any airgaps are introduced, then further calculations must be made which considers these airgaps.
Every document cited herein, including any cross referenced or related patent or application and any patent application or patent to which this application claims priority or benefit thereof, is hereby incorporated herein by reference in its entirety unless expressly excluded or otherwise limited. The citation of any document is not an admission that it is prior art with respect to any invention disclosed or claimed herein or that it alone, or in any combination with any other reference or references, teaches, suggests or discloses any such invention. Further, to the extent that any meaning or definition of a term in this document conflicts with any meaning or definition of the same term in a document incorporated by reference, the meaning or definition assigned to that term in this document shall govern.
While the present invention has been illustrated by a description of one or more embodiments thereof and while these embodiments have been described in considerable detail, they are not intended to restrict or in any way limit the scope of the appended claims to such detail. Additional advantages and modifications will readily appear to those skilled in the art. The invention in its broader aspects is therefore not limited to the specific details, representative apparatus and method, and illustrative examples shown and described. Accordingly, departures may be made from such details without departing from the scope of the general inventive concept.
The present application claims priority to U.S. Provisional Application Ser. No. 63/284,139 filed Nov. 30, 2021, the contents of which is hereby incorporated by reference in their entry.
The invention described herein may be manufactured and used by or for the Government of the United States for all governmental purposes without the payment of any royalty.
Number | Date | Country | |
---|---|---|---|
63284139 | Nov 2021 | US |