Liquid purification or separation – Processes – Chromatography
Reexamination Certificate
2002-06-10
2004-03-02
Therkorn, Ernest G. (Department: 1723)
Liquid purification or separation
Processes
Chromatography
C210S198200, C095S082000, C096S101000
Reexamination Certificate
active
06699392
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates generally to microfabricated silicon chromatographic columns, and more specifically to methods to fabricate microfabricated silicon chromatographic columns with through-substrate fluid ports.
BACKGROUND OF THE INVENTION
Chromatographic columns are an important part of many chemical and biological detector systems. Prior art chromatographic columns have been manufactured in silicon substrates using techniques closely related to those of the integrated circuit industry.
A prior art silicon chromatographic column is shown in FIG.
1
. In such prior art silicon chromatographic columns, a Bosch-etched trough
101
, typically in the shape of a spiral with a rectangular cross-section, is formed in a silicon substrate
100
. The trough is typically some tens of microns in width, some hundreds of microns in depth, and has a total length on the order of a meter. A thin stationary phase (not shown) can be added to the surface of the trough to enhance the separating properties of the final chromatographic column. The open side of the trough is then typically covered with a glass lid
102
, thereby converting the trough into a long spiral column. The glass lid is often composed essentially of a Pyrex glass. The glass lid can be bonded to the silicon substrate using a variety of techniques, but is preferentially attached by anodic bonding.
Note that the glass lid
102
is shown as considerably thicker than is silicon substrate
100
. This is typical of this type of prior art chromatographic column. The silicon substrate is significantly weakened by the formation of the trough
101
, and the additional thickness of the glass lid is needed to obtain a product sufficiently robust for the desired applications. In this example, fluid access to the spiral column is provided by access ports
103
and
104
which penetrate glass lid
102
.
Such a prior art silicon chromatographic column has multiple advantages over more conventional chromatographic columns, which typically take the form of millimeter-diameter tubes having a length of several meters. For example, whereas a conventional gas chromatograph can ramp in temperature at a typical rate of 10-20° C. per minute, this requires a heater power of hundreds of watts. The prior art silicon chromatographic columns can ramp in temperature an order of magnitude more rapidly with a heater input which is two orders of magnitude smaller. Such columns enable a rapid, portable, and low-power detector.
However, prior art silicon chromatographic columns can be improved upon. For structural integrity and ease of manufacture, the glass lid must be rather thick, typically on the order of a millimeter. As a result, the glass lid is usually the largest contributor to the heat capacity of the silicon chromatographic column. In addition, the prior art silicon chromatographic column has an extremely large surface area to volume ratio, owing to the flat and single-layer configuration. Both these features act to increase the power requirements of a detector system which comprises such columns.
An additional limitation of prior art chromatographic columns is their column length. While sufficient for some purposes, for others a column length considerably in excess of one meter is beneficial. Typical conventional gas chromatographs, for example, have column lengths of about 5-20 meters.
All of the above concerns can be addressed by forming an interconnecting stack of silicon chromatographic columns. The stacking of individual silicon chromatographic columns atop each other allows thinner glass lids to be used between them, as such a stack is stronger than is an individual silicon chromatographic column. As a result, the heat capacity of the stacked columns is less than the heat capacity of the same number of columns which are not stacked. Formation of a stack also favorably alters the surface area to volume ratio, thereby reducing average heat losses to the environment.
Finally, if the individual silicon chromatographic columns are properly interconnected, it is possible to form a longer combined column. Alternately, it is possible to connect several columns in parallel, each column having access to the same sample material. In this case, the aim can be to increase throughput of the chromatograph, or can be to perform several different chromatographic separations simultaneously.
Successfully forming such a stack of individual silicon chromatographic columns is a task made easier if fluid ports can be formed through the silicon substrate, thus allowing interconnections between the columns to be made within the material of the stack. Alternate procedures involve making external connections between the individual silicon chromatographic columns, and such connections are both difficult to make and lack physical robustness. A minimum of two through-substrate fluid ports are required for each individual silicon chromatographic column: one at the inlet of the column and the other at the output of the column.
FIG. 2
shows an individual silicon chromatographic column with multiple fluid ports. Chromatographic trough
201
is fabricated in a first surface of silicon substrate
200
. Through-substrate fluid ports
202
,
203
,
204
, and
205
provide access to the outer part of chromatographic trough
201
, while through-substrate fluid port
206
provides access to the inner part of chromatographic trough
201
. A glass lid (not shown) is then placed atop said first surface of silicon substrate
200
to convert chromatographic trough
201
into a chromatographic column. Access to said chromatographic column can be obtained through fluid ports
202
-
206
, as needed for a particular application.
An implementation of a stack comprising two levels of individual silicon chromatographic columns is shown in FIG.
3
. Here fluid input
300
provides access to fluid port
303
in first silicon chromatographic column
302
. Fluid port
303
connects to the outer portion of first chromatographic trough
304
. Fluid port
305
does not connect to first chromatographic trough
304
, but rather pierces first silicon chromatographic column
302
. Fluid output
301
connects to fluid port
305
.
Pyrex cap
306
is affixed atop first silicon chromatographic column
302
, so that cap port
307
connects to the central portion of first chromatographic trough
304
. Cap port
308
is positioned so that it connects to fluid port
305
.
Second silicon chromatographic column
309
, which comprises second chromatographic trough
310
is affixed atop Pyrex cap
306
. Fluid port
311
is formed so that it connects to the central portion of second chromatographic trough
310
and to cap port
307
. Fluid port
312
is formed so that it connects to the outer portion of second chromatographic trough
304
and to cap port
308
. Finally, Pyrex cap
313
is affixed atop second silicon chromatographic column
309
.
In use, carrier fluid is pumped into fluid input
300
. The fluid then passes through the length of first chromatographic trough
304
, which has been converted into a chromatographic column by the affixing of Pyrex cap
306
. The fluid then passes through cap port
307
in Pyrex cap
306
, and then into second chromatographic trough
310
through fluid port
311
. The fluid passes through the length of second chromatographic trough
310
, then passes through fluid port
312
, cap port
308
, and fluid port
305
to exit the stacked chromatographic structure through fluid output
301
. The fluid passing through fluid output
301
is ten directed to the desired detection, separation, or collection apparatus, which is not shown.
Due to the crystal structure of silicon and the high aspect-ratio of the desired spiral chromatographic trench, the trench must be fabricated in the silicon substrate using Bosch etching. The fluid ports can be formed using Bosch etching or wet etching, but are beneficially formed prior to the Bosch etching of the spiral chromatographic trench.
However, Bosch etching uses helium cooling gas on the side of the silicon subst
Adkins Douglas R.
Frye-Mason Gregory C.
Heller Edwin J.
Manginell Ronald P.
Dodson Brian W.
Sandia Corporation
Therkorn Ernest G.
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