Process for fiberizing ceramic materials with high fusion temperatures and tensile strengt

Gates, L. E., Jr.

Lent, W. E.

English

NASA Technical Reports Server

REPLY TO 
ATTN OF: March 27 ,  1971 
TO : 
FROM : 
SUBJECT : 
USI/Scientific & Technical Information Division 
Attention: Miss Winnie M. Morgan 
GP/Office of Assistant General 
Counsel for Patent Matters 
Announcement of NASA-Owned 
U.S. Patents in STAR 
In accordance with the procedures contained in the Code GP 
to Code US1 memorandum on this subject, dated June 8, 1970, 
the attached NASA-owned U.S. patent is being forwarded for 
abstracting and announcement in NASA STAR. 
The following information is provided: 
U.S. Patent No. : 3,337,315 
Hu hes Aircraft Company 
Corporate Source : Cu 7 ver City, California 
Supplementary 
Corporate Source 
NASA Patent Case No.: XNP-00597 
Please note that this patent covers an invention made by an 
employee of a NASA contractor. 
the National Aeronautics and Space Act, the name of the 
Administrator of NASA appears on the first page of the patent; 
however, the name of the actual inventor (author) appears at 
the heading of Column No. 1 of the Specification, following the 
words I@.  . . with respect to an invention of. . e . I 1  
Pursuant to Section 305(a) of 
https://ntrs.nasa.gov/search.jsp?R=19710013612 2020-03-17T03:00:21+00:00Z
JAMES E. WEBB 3,337,315 
ADMINtSTRATOR OF THE NATlONAL AERONAUTICS 
A N D  SPACE ADMINISIRATtON 
METHOD FOR FIBERIZING CERMIC MATERIALS Fila-d Nor. 10. 1964 I .-- - -- 
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into fabrics or rigid structural components 
which are remarkably resistant to heat. 
The prior art fails to teach two or more of the afore- 
mentioned process steps. A typical example of a process 
5 for fiberizing materials re€ies on the materials initially be- 
ing iii a liquid state, and in this conditiot the material 
is blasted by jets of gas. The likelihood of obtaining gfob- 
ules or unSberized contaminacts mixed with the glass 
fibers is excellent. 
Another typical prior art example employs the hori- 
zontal process for fiberizing materials. A horizontally held 
ceramic rod is heated and simultaneously fiberized, there 
ntrd of the ceramic viscosity. Since viscosity 
control is absent the material flows away from the blast- 
the viscosity is such as to preclude obtaining 
Another example of prior art deficiency uses blasting 
jets of gas which are not precisely directed at the ma- 
terial, thereby resulting in reducing the fiber yield. 
The prior art also fails to teach the use of tempera- 
tures required for melting refractory glasses together with 
the precise control over the temperature of molten ma- 
terial to achieve efficiency in converting the molten ma- 
terial into usable fibers. 
The foregoing and other advantages of the process 
invention and materials employable therewith will be- 
come more apparent from a consideration which follows 
taken in conjunction with the drawings. 
10 
42 USC 2457). 
This invention relates to a process for fiberizing ceramic 
materials, and it further relates to materials suitable for 
fiberking. 
ith tbe increasing need both in industry and govern- 
ment for ceramic materials having relatively high fusion 
te~peratures and tensile strengths, the effort to obtain 
such materials and a process to fiberke the same has in- 
which will provide adequate protection to individuals and 
critical aerospace corn nents are in considerable demand 
in the aerospace industry. ing in heat 
hazardous areas need adequate PrOwVe ClothinS, and 
m ~ h a n ~ c a l  oomponents, proximate to the high tempera- 30 for f ibedng  ceramic materials; 
20 
r instance, heat resistant types of materials 23 
FIG. 1 is a schematic drawing austrating the pr 
Zonm of rocket engines, to fabricated of FIG. 2 is an enlarged sectional view partially in eleva- 
tion, illustrating, in solid lines, the position of the ceramic 
rod surrounded by an annular ring nozzle, and the loca- 
tion of the lower heated end of the rod with respect to 
FIG. 3 i s  a plan view, partially in section, taken on 
line 3-3 of FIG. 2. 
the absence of suitable materials these components 
are destroyed or subject to destruction which may very 
well result in aborting and delaying a program until the " the direction of flow of the bursts of gas jets: and 
damage is repaired. 
The aforementioned increased effort has produced the 
r described prwess and materials. 
The process 
time between steps ( I )  and ( 5 )  lo  achieve optimum vis- 
cosig of the material. 
foregoing process, are uniquely formulated to provide for 
relatively high fusion temperatures and tensile strengths. 
which may be 
With ceramic rod I@ heid in the solid line position illus- 
trated in FIG. 1, the Iower end thereof is located between 
gized produce sufficient heat to achieve melting of the 
lower end of the ceramic rod. The rotation of rod 
homogenous molten droplet 
n e  ceramic materials, suitable to be fiberizecf by the 60 a pair of spaced carbon electrodes 2 
n properly treated by ~e materials pro- gether with the heating produces a relatively uniform 
ide a relatively high yield of 
1 I_-------_-- 
6 _____________ 
6 _____________ 
10 ----------- 
xample 9 is employed for the p 
viscosity of ceramic material when 
pendence of these two parameters upon time. The re- while at the same time contributing to the attainment of 
quired cooling rate immediately after the fibers are fomed a high fiber yield. 
is dependent upon the rate at which the fiber solidifies. 
The gas employed may be air, steam or other gases 10 has been determined to be 267,000 pounddsquare 
inert to the ceramic material. 65 inch, and the mean tensile strength of Example 11 has 
The burst of gas striking molten droplet will pro- been determined to be 295,000 pomds/square inch. 
duce fibers of the material which can then be collected 
and used to weave materials having the aforementioned with Capa acting as the mdfier.  One school of thought 
physical properties. Rigid components having relatively indicates the larger diameter of the fluoride anion is re- 
high fusion temperatures and tensile strengths may be 70 sponsible for its ability to aid in glass network forming 
fabricated by combining the fibers With a suitable bider. believing it promotes a @eater stab of disorder which 
After the maximum yield of fibers is obtained from is responsible for grass formation. 
In the case of Example 11 of the itemized tist, it has 
process repeated. This procedure may be followed until optimum molar ratb is 1 : 1- 
1, 3, 4 and 10 it has been deter& 
The mean tensile strength of 
MZO3 is considered the glass former in 
75 
best results may be achie by maintaining the molar 
ratio of A&& to MgO of 3: 1. 
If thc ceramic comp&tions am those listed in Table 
it is to be noted the aforementioned delay time occur- 
ring between step or phase 1 and phase or step 5 of 
the process varies between 0.5-3 seconds, and 50 blasts 
of gas pressurized to 300 pounds per square inch pro- 
duws the yield and fiber texture indicated 
$yntk&ing the ceramic rads is accomplished in the 
following manner: Chemically pure oxides are accurately 
weighed and blended in a countercurrent batch mixer 
with water and snssCient organic binder to produce ex- 
trusion consistency. Extrusion is  performed through a H 
inch diameter vacuum die with the aid of 8 hydraulic 
press. The eight-inch-long rods produced are then dried 
and sintered in air to 1250" C. A sintered rod can then 
be fiberized using the aforementioned process. 
while the inventions have been described herein in 
what is considered preferred embodiments, it should be 
recognized departures may be made therefrom within 
the scope of the inventions, and the inventions should 
therefore not k limited to the details of the w&in dis- 
closures, but should be accorded the full scope of the 
appended claims. 
What is claimed is: . A method of fiberizing ceramic materials to achieve 
a relatively high yield of fibers comprising: 
(a) heating one end of an elongated ceramic rod un- 
til a relatively uniform homogeneous molten droplet 
f o m  on the heated end thereof; 
(b) moving said rod from the heat mne to a position 
'prorimate to annular ring nozzle; 
(c) moving said rod and ring nozzle relative to ea& 
droplet portion of the e e d c  rod, and 
directed jets of pressurized gas. 
(d) fiberizing the droplet with inclined do 
2. A method of fiberizing ceramic materials according 
to claim 1 wherein said ceramic rod, in step (a) is ro- 
tated about the longitudinal axis while Wig heated to 
achieve obtaining a relatively uniform homogeneous mol- 
ten droplet. 
3. A method of fiberizing ceramic materials accord- '' ing to claim 1 wherein the apex of the gas jets form a sub- 
stantially acute angle with the longitudinal axi3 of said 
ceramic rod, the acute angle being between about 25' 
and 50". 
4. A method of fiberizing ceramic materials according 
to claim 1 wherein said gas in step (d) is pressurized be- 
tween approximately 2SO and 350 pounds per square inch. 
5. A method of fiberizing ceramic materiah to &$eve 
a relatively high yield of fibers comprising: 
(a) rotating a verticalty held elongated ceramk rod 
in a heat zone until a relatively uniform homogene- 
ous molten droplet forms on the lower end 
(b) moving said rod from the heat zone to a 
proximate to an annular ring &e where 
(e) moving said rod and ring node relative to 
other whereby the ring nozzle surrounds the molten 
dropiet portion of the ceramic rod, and 
(d) fiberizing the droplet with inclined downwardly 
directed jets of pressurized gas, there being a h g  
time from achieving the molten droplet of step (a) 
to fiberizing the droplet of step (d) between abut  
0-5 seconds to achieve optimum viscosity of 
droplet to obtain the maximum fiber yield, 
g 
15 
go 
e6 oftherodceases; - 
80 
2,133,236 
2,175,224 
2,822,579 
2,881,471 
2,916.773 
2,984,868 
2,987,733 
45 3,099,548 
UNITED STATES PATENTS 
IO11938 Slayter et d. ______ 
1011939 Slayter ___________ 
211958 Silverman _____c___ 
411959 Snow et al. _-_____ 
1211959 Vonnegut. 
3/1961 IIiu ______________ 
611963 Stalego ___________ 
711963 Ducati ----__-_____ 
FOREIGN PATENTS 
180,739 1/1955 Germany. 
R LINDSAYa Asdrtant E e r ,  
@ DON= E. SYLVESTER, Primary Examiner. 


Method for fiberizing ceramic materials Patent

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