CN107703054B - A kind of measuring device and method of gel macroscopic adhesion forces - Google Patents
A kind of measuring device and method of gel macroscopic adhesion forces Download PDFInfo
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- CN107703054B CN107703054B CN201710916930.5A CN201710916930A CN107703054B CN 107703054 B CN107703054 B CN 107703054B CN 201710916930 A CN201710916930 A CN 201710916930A CN 107703054 B CN107703054 B CN 107703054B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
Abstract
The invention discloses the measuring devices and method of a kind of gel macroscopic adhesion forces.The measuring device includes pedestal and upper cover, and the upper cover is covered on the pedestal and forms accommodation space；Opposite watch window there are two being set on the side wall of the pedestal；The upper lid is equipped with a through-hole, and a cylinder is hung on the upper lid by the through-hole, and the other end of the cylinder extends to the position corresponding position of the watch window.After measurement gel solution and unlike material matrix attachment contact plastic that the measuring device of inventive gel macroscopic adhesion forces can quantify, the macroscopical peel adhesion occurred between gel and contacting substrate, and the adherency difference between gel and unlike material contacting substrate can be compared, this is not only drilled gel valve during well to oil field underbalance, and pressure-resistant technique is implemented with great directive function at the scene, it may also be used for the evaluation of the gel macroscopic adhesion forces of general field.
Description
Technical field
The present invention relates to the measuring device and method of a kind of gel macroscopic adhesion forces, the adhesion strength for belonging to high-strength gel is surveyed
Amount field.
Background technique
It is drilled in well in underbalance using pressure-resistant technique gel valve, one section is vacantly formed in casing has mechanical strength
High viscosity gels slug, gel slug block pit shaft using the mechanical strength of its own and with the adhesiveness of contact tube wall with flat
Weigh strata pressure, to prevent oil gas from revealing, while avoiding pollution of the overbalance operation to reservoir caused by drilling well and well killing fluid,
Have the function of isolation, sealing and pressure-bearing, and the pressure-resistant performance for improving gel valve prevents it from breaking through the machine that must just improve frozen glue
Tool intensity and adhesiveness.There are many characterizing method of frozen glue mechanical strength at present, and the means for the measurement adhesiveness relatively approved are to utilize
Atomic force microscope (AFM) measures microcosmic adhesion strength (μ N), but not yet finds the test method and suitable measuring device of system
Macroscopic adhesion forces are measured, accordingly, it is desirable to provide a kind of device and method for measuring macroscopic adhesion forces.
Summary of the invention
The object of the present invention is to provide the measuring device and method of a kind of gel macroscopic adhesion forces, macroscopic adhesion forces, that is, fluid
The adhesion strength that adherency removing occurs after plastic between contacting substrate, by cooperating with Texture instrument, apparatus of the present invention can be surveyed quantitatively
The macroscopic adhesion forces between gel and contacting substrate are measured, can be used for investigating the influence factor of gel adhesion strength power, and be capable of measuring solidifying
The adhesion strength difference of glue and different contact materials uses progress directive function to the kill-job of gel valve at the scene.
The measuring device of gel macroscopic adhesion forces provided by the present invention, including pedestal and upper cover, the upper cover are covered on
Accommodation space is formed on the pedestal；
Opposite watch window there are two being set on the side wall of the pedestal；
The upper lid is equipped with a through-hole, and a cylinder is hung on the upper lid by the through-hole, and the cylinder
The other end extends to the position corresponding position of the watch window.
In the measuring device of the gel macroscopic adhesion forces, the internal diameter of the pedestal can be 25~85mm, highly can be
30~80mm；
The internal diameter of the upper cover can be 25~85mm, highly can be 25~60mm；
The diameter and height of the cylinder can be 20~80mm.
It is detachably to cooperate between the pedestal and the upper cover in the measuring device of the gel macroscopic adhesion forces,
It is concretely threadedly engaged, the cylinder being set on the upper lid can be made by screw thread and is held in the pedestal solidifying
Glue realizes critical interfaces contact.
In the measuring device of the gel macroscopic adhesion forces, the watch window is set to the opening of the pedestal, leads to
The standoff distance between the gel liquid in the pedestal and upper the part cylinder can be observed and connect by crossing the watch window
Touching degree.
In the measuring device of the gel macroscopic adhesion forces, the cylinder hangs on institute by the outer that its end is arranged
It states on lid, realizes that the cylinder is successfully equipped on the upper cover, and the cylinder outer wall realizes that zero rubs with the upper cover inner wall
Contact is wiped, and in measurement process, the cylinder carries upwards to be influenced by the upper cover.
In the measuring device of the gel macroscopic adhesion forces, the watch window is symmetrical set, and guarantees the transmission of light,
It is capable of the contact of accurate observation liquid level and cylinder bottom when containing coagulant liquid toward pedestal.
In the measuring device of the gel macroscopic adhesion forces, the pedestal, the upper cover and the cylinder are in cylinder
The bodily form.
The material of the pedestal, the upper cover and the cylinder is stainless steel, polytetrafluoroethylene (PTFE) or organic glass etc.；
Wherein, carbon steel material of the stainless steel close to casing on site；Visual testing can be carried out using lucite tube；It is poly-
Tetrafluoroethene material has high lubrication and non-stickiness, and category hates liquid (water) material；It therefore can be by being glued on above-mentioned three kinds of contacting substrates
The measurement and comparison of attached property, and then the adhesiveness of quantitative assessment (compound) gel.
In the gel adherency force measuring device, the upper surface of the cylinder is equipped with a hanged hook or is connected by a body of rod
Connect a hanged hook, when measurement, hung up the cylinder by the hanged hook, i.e., by the hanged hook by the cylinder from institute
It states and is removed on gel.
The body of rod can be embedded in the column body by way of being threadedly engaged.
In the gel adherency force measuring device, the size of the pedestal, the upper cover and the cylinder can be according to need
It is adjusted.
The measuring device of gel macroscopic adhesion forces of the present invention can cooperate with Texture instrument, realize to gel adhesion strength
Measurement；It can be carried out as steps described below when specific measurement: gel solution is placed in the measuring device of the gel macroscopic adhesion forces
The pedestal in, then by the upper cover and the base engagement, make the gel solution upper surface and the cylinder
Following table face contact (just contacts)；After the gel plastic, using the Texture instrument measure the gel and the cylinder it
Between adhesion strength；In measurement process, under the drive of strength induction member, the column vertical is at the uniform velocity moved up, the gel
It is bent to obtain adhesion strength measurement by computer record for the adhesion strength generated with the whole process that the cylinders contact matrix separates at any time
Line.
The measurement gel solution and unlike material matrix attachment that the measuring device of inventive gel macroscopic adhesion forces can quantify
After contacting plastic, the macroscopical peel adhesion occurred between gel and contacting substrate, and gel and unlike material contact base can be compared
Adherency difference between matter, this not only to oil field underbalance be drilled gel valve during well at the scene pressure-resistant technique be implemented with it is great
Directive function, it may also be used for the evaluation of the gel macroscopic adhesion forces of general field.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that inventive gel adheres to force measuring device.
Fig. 2 is the structural schematic diagram that inventive gel adheres to force measuring device and Texture instrument cooperation.
It is respectively marked in figure as follows:
1 pedestal, 2 upper covers, 3 watch windows, 4 cylindrical bodies, 5 bodies of rod, 6 Texture instruments.
Fig. 3 is that adhesion strength changes over time curve between silica plural gel and stainless steel in the embodiment of the present invention 2.
Fig. 4 is that adhesion strength changes over time between 5wt% silica plural gel and stainless steel in the embodiment of the present invention 2
Curve.
Fig. 5 is that the adhesion strength in the embodiment of the present invention 2 between silica plural gel and polytetrafluoroethylene (PTFE) becomes at any time
Change curve.
Fig. 6 is that adhesion strength is at any time between 10wt% silica plural gel and organic glass in the embodiment of the present invention 2
Change curve.
Fig. 7 is the adhesion strength comparison diagram of silica plural gel and different contacting substrates in the embodiment of the present invention 2.
Fig. 8 is that the adhesion strength in the embodiment of the present invention 2 between montmorillonite Composite gel and stainless steel changes over time curve.
Fig. 9 is that the adhesion strength in the embodiment of the present invention 2 between montmorillonite Composite gel and organic glass changes over time song
Line.
Figure 10 is that the adhesion strength in the embodiment of the present invention 2 between montmorillonite Composite gel and polytetrafluoroethylene (PTFE) changes over time
Curve.
Figure 11 is the adhesion strength comparison diagram of montmorillonite Composite gel and different contacting substrates in the embodiment of the present invention 2.
Figure 12 is that the adhesion strength in the embodiment of the present invention 2 between starch plural gel and stainless steel changes over time curve.
Figure 13 is that the adhesion strength in the embodiment of the present invention 2 between starch plural gel and polytetrafluoroethylene (PTFE) changes over time song
Line.
Figure 14 is that the adhesion strength in the embodiment of the present invention 2 between the compound solidifying organic glass of starch changes over time curve.
Figure 15 is the adhesion strength comparison diagram of starch plural gel and different contacting substrates in the embodiment of the present invention 2.
Figure 16 is the adhesion strength comparison diagram of different composite gel and stainless steel contacting substrate in the embodiment of the present invention 2.
Figure 17 is the adhesion strength comparison diagram of different composite gel and organic glass contacting substrate in the embodiment of the present invention 2.
Figure 18 is the adhesion strength comparison diagram of different composite gel and polytetrafluoroethylene (PTFE) contacting substrate in the embodiment of the present invention 2.
Figure 19 is contacting substrate surface microstructure in the embodiment of the present invention 2, and wherein Figure 19 (a) is that the face of stainless steel is microcosmic
Structure, Figure 19 (b) are the face microstructure of organic glass；Figure 19 (c) is the face microstructure of polytetrafluoroethylene (PTFE).
Figure 20 is that drop spreads balance schematic diagram.
Figure 21 is that gel breaks through mode in pipe, and wherein Figure 21 (a) is interior bubble, and Figure 21 (b) is that entirety moves up, Figure 21
(c) it is broken through between tube wall.
Figure 22 is the adhesion strength in the embodiment of the present invention 2 between different composite gel and stainless steel rotor (cylindrical body).
Figure 23 is the adherency in the embodiment of the present invention 2 between different composite gel and polytetrafluoroethylene (PTFE) rotor (cylindrical body)
Power.
Figure 24 is the adhesion strength in the embodiment of the present invention 2 between different composite gel and organic glass rotor (cylindrical body).
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1, gel adhere to force measuring device
As shown in Figure 1, the structural schematic diagram of the measuring device for inventive gel macroscopic adhesion forces, it includes 1 He of pedestal
Upper cover 2, pedestal 1 and upper cover 2 are in cylindrical, and pedestal 1 and upper cover 2 can be by being threadedly engaged and forming accommodation space.Its
In, it is highly 50mm that the internal diameter of pedestal 1, which is 60mm, and it is highly 35mm that the internal diameter of upper cover 2, which is 60mm,.It is set on the side wall of pedestal 1
There are 2 symmetrical watch windows 3, and watch window 3 is set to the opening of pedestal 1.Upper cover 2 is equipped with a circular through hole (figure
In do not mark), a cylindrical body 4 is hung in upper cover 2 by circular through hole, and the other end of cylindrical body 4 extends to watch window 3
Position corresponding position, i.e., the lower end of cylindrical body 4 is able to observe that by watch window 3, the diameter and height of cylindrical body 4 are
50mm.In the present invention, the outer (not marking in figure) that cylindrical body 5 is arranged by upper end is hung in upper cover 2.Edge in cylindrical body 4
It is axially arranged with a body of rod 5, and the body of rod 5 is set in cylindrical body 4 by way of being threadedly engaged, and the free-end of the body of rod 5 is equipped with outstanding
Hook.
Inventive gel adheres in force measuring device, and the size of pedestal 1, upper cover 2 and cylindrical body 4 can be adjusted as needed
It is whole.
In the measuring device of inventive gel macroscopic adhesion forces, the material of pedestal 1, upper cover 2 and cylindrical body 4 may be selected stainless
Steel, polytetrafluoroethylene (PTFE) or organic glass etc., wherein carbon steel material of the stainless steel close to casing on site；Using lucite tube
It can carry out visual testing；Polytetrafluoroethylene (PTFE) material has high lubrication and non-stickiness, and category hates liquid (water) material；It therefore can be by upper
State the measurement and comparison of adhesiveness on three kinds of contacting substrates, and then the adhesiveness of quantitative assessment (compound) gel.
As shown in Fig. 2, the measuring device of inventive gel macroscopic adhesion forces can be cooperated with Texture instrument 6, realization pair
The measurement of gel adhesion strength.It can be carried out as steps described below when specific measurement: gel solution is placed in gel adhesion strength measurement dress
In the pedestal 1 set, then upper cover 2 and pedestal 1 are cooperated, connect the upper surface of gel and the following table face contact of cylindrical body 4 (just
Touching)；After gel plastic, the adhesion strength between gel and cylindrical body 4 is measured using Texture instrument 2；In measurement process, in strength sense
Under the drive of Ying Yuan, cylindrical body 4 is vertically at the uniform velocity moved up, the entire mistake that gel separates at any time with 5 contacting substrate of cylindrical body
The adhesion strength that journey generates, obtains adhesion strength experiment curv by computer record.
The application of embodiment 2, gel adherency force measuring device
One, between plural gel and contacting substrate adhesion strength quantitative determination
About 100g plural gel is taken to pour into the pedestal 1 of the measuring device of the gel macroscopic adhesion forces of embodiment 1.It will have
The upper cover 2 of cylindrical body 4 is slowly contacted by the rotation of screw thread with 1 part of pedestal, and the watch window 3 on the side wall of pedestal 1 is passed through
Observation coagulant liquid is just contacted with the cylindrical body 4 of upper part, is measured entire gel adhesion strength with adhesive tape and preservative film and is filled
Sealing is set, is placed in 70 DEG C of thermostatic drying chambers and reacts, crosslinking is taken out afterwards for 24 hours, is removed adhesive tape and preservative film, is connected with Texture instrument
It measures the plural gel and contacts the adhesion strength between rotor (cylindrical body 4).
Adhesion strength quantitative determination in, composite gel system by 2wt% polyacrylamide, 0.2wt% chromium acetate,
The thiocarbamide and concentration of 0.2wt% is respectively that the reinforcing agent of 0wt%, 1wt%, 3wt%, 5wt%, 7wt% and 10wt% (cover de-
Soil, silica and starch) composition, as shown in table 1, this formula plastic at 70 DEG C takes out measurement to formula afterwards for 24 hours.
The formula of 1 composite gel system of table
1, the adhesion strength of silica plural gel
The adhesion strength of silica plural gel and stainless steel contacting substrate changes over time curve such as Fig. 3, and adhesion strength is surveyed
Amount curve is divided into three phases, such as Fig. 4, it can be seen that (a-b) in the first stage, the stainless steel with plural gel adhesion contact
When cylinder top half is at the uniform velocity lifted upwards under the action of Texture instrument tension belt, the stainless steel cylinder that is adhered to each other originally
It tears and separates with plural gel, strength induction member senses gel that cylinder is subject to its downward adhesion strength, with drawing
The increase of distance is stretched, this power is gradually increased；The stainless steel cylinder of second stage (b), plural gel and adhesion contact is peeling-off
Moment, the member of strength induction at this time senses the cylinder maximum adhesion power downward by gel, therefore adheres to force curve and reach most
Big value；Phase III (b-c), stainless steel cylinder are gradually disengaged with gel, and the adhesion strength for the latter that the former is subject to is smaller and smaller, are glued
Attached force curve is gradually reduced the final weight to stainless steel rotor and connecting screw.From the figure 3, it may be seen that silica concentration is to compound
Gel adhesion strength has significant impact.Adherency with the increase of silica concentration, between plural gel and stainless steel contact surface
Power shows a increasing trend.This and nano silica are related with the molecular force of stainless steel stromal surface.Stainless steel surface is due to Fe-OH
With the distribution presence-OH group of iron oxide, and there are three kinds of different bond styles for the nano-silica surface of large specific surface area
Hydroxyl, be single raw silicone hydroxyl respectively, adhesion is associated silicone hydroxyl and twin silicone hydroxyl, when nano silica plural gel with not
When steel surface of becoming rusty contact, in addition to polymer chain, the active force of water and stainless steel surface, nano-silicon dioxide particle and stainless steel watch
- the OH in face forms intermolecular hydrogen bonding, and nano-silicon dioxide particle concentration is higher, mentions with the hydrogen bond quantity of stainless steel watch face contact
The caking property of height, plural gel and stainless steel surface is reinforced, therefore the adhesion strength between the two is with nano silica ion concentration
Increase and increase.
Fig. 5 and Fig. 6 is respectively the adhesion strength experiment curv between plural gel and polytetrafluoroethylene (PTFE), organic glass.It can by figure
Know, with the increase of silica concentration, the adhesion strength between plural gel and contacting substrate is gradually increasing, except that adherency
The difference of power.The maximum value of adhesion strength between plural gel and contacting substrate under various concentration, i.e. peak value in Fig. 2 curve are taken respectively
B is individually subtracted the weight with the matrix rotor of gel contacts, obtains the adhesion strength between plural gel and unlike material contacting substrate
Difference.Be 0wt%~3wt% in particle concentration section such as Fig. 7, silica plural gel respectively with stainless steel and organic glass
The peel adhesion of glass is not much different, but works as particle concentration and increase to 10wt% from 5wt%, the peel adhesion between organic glass
Power is respectively 23.839N, 25.184N and 40.930N, and the adhesion strength between stainless steel is respectively 19.998N, 22.521N and
33.066N, the adhesion strength between plural gel and organic glass are slightly larger than stainless steel.
2, the adhesion strength of montmorillonite Composite gel
Fig. 8-Figure 11 is respectively between montmorillonite Composite gel and stainless steel, organic glass and polytetrafluoroethylene (PTFE) contacting substrate
Separate adhesion strength test curve.As seen from the figure with the increase of particle concentration, between plural gel and stainless steel and organic glass
Separation adhesion strength is gradually increased, and the adhesion strength variation between polytetrafluoroethylene (PTFE) is little.Because the piece layer architecture surface of montmorillonite has
Have a certain number of hydroxyls, and surface is negatively charged, when being contacted with stromal surface, respectively with the-OH of stainless steel surface, organic glass
- C-O and the O-C=O group on glass (polymethyl methacrylate) surface generate molecular link, with the increase of particle concentration, molecule
The quantity of key increases, and the bonding point intensity of plural gel and stromal surface increases.Polytetrafluoroethylene (PTFE) is the nonpolarity of high degree of symmetry
High molecular material has excellent thermal stability, and there are faint dispersion forces between montmorillonite, therefore with montmorillonite concentration
Increase, the adhesion strength amplitude of variation between plural gel and polytetrafluoroethylene (PTFE) is smaller.
Adherency removing curve discovery between low concentration and high concentration montmorillonite Composite gel and contacting substrate is compared, in montmorillonite
When low concentration, plural gel and the peeling-off required time of contacting substrate are longer, and such as Fig. 8, not plus montmorillonite Composite gel occurs
The time of removing is higher than 70s, and 1wt% montmorillonite Composite gel is peeling-off to need 55s, with the increasing of reinforcing agent particle concentration
Greatly, the plural gel time peeling-off with contacting substrate is gradually shortened, 10wt% montmorillonite Composite gel and contacting substrate
Removing occurs within 5s.In influence of fourth, fifth, the six chapters research reinforcing agent particle to performance, it has been found that plural gel is viscous
Elasticity increases with the increase of particle concentration, and plural gel is usually accompanied by during separating with contacting substrate and coagulates
The draw stage of glue after gel stretches to a certain extent, occurs adherency with contacting substrate and separates.It therefore deduces that, particle is dense
Degree is lower, and the level of stretch between plural gel and contacting substrate is bigger, corresponding longer the time required to separation；And particle concentration is high
When, level of stretch is low between gel and matrix, and separating rate is very fast.The reason is that for the plural gel under low concentration (≤3wt%),
The contact that the biggish mobility of system and morphotropism support it relatively good with stromal surface causes tight between gel and contacting substrate
Close adherency, and the elasticity of plural gel ontology is weaker, therefore gel is incited somebody to action when by with the stretching of its contact cylinder adhered to
First occur one section of long period elastic stretching, later elastic stretching greatly to a certain extent after, gel just and contacting substrate occur
Removing.And for high concentration (5wt%~10wt%) plural gel, although there is also elastic stretching, it is solidifying compared to compound
The elastic strength of glue itself, be easier with the adhesiveness of contacting substrate it is first peeling-off, therefore high concentration plural gel by
When to the stretching of its contact cylinder adhered to, elastic stretching by a small margin occurs for ontology and matrix is peeling-off, splitting time
Comparatively fast.As shown in Figure 11, the peel adhesion difference between montmorillonite Composite gel contacting substrate different from three kinds is larger, wherein with
Peel adhesion between organic glass matrix is maximum, reaches as high as 35.701N, the followed by adherency with stainless steel contacting substrate
Peel adhesion of the peel adhesion of power, 10wt% montmorillonite Composite gel and stainless steel between 10.335N, with polytetrafluoroethylene (PTFE)
Power is minimum, and influence of the increase of particle concentration to its adhesion strength is smaller.Illustrate the pairs of plural gel of the group of contacting substrate
Adhesion strength influences very big.
3, the adhesion strength of starch plural gel
Figure 12-Figure 15 is that the adhesion strength of starch plural gel contacting substrate different from three kinds removes experiment curv.It can by figure
Know, with the increase of starch concentration, the adhesion strength between plural gel and stainless steel and organic glass is gradually increased, with polytetrafluoro
Adhesion strength between ethylene has almost no change.This is similar with the enhancing trend of silica and montmorillonite particle.Due to amylum body
Hydroxyl-the OH and stainless steel and the group on organic glass surface on sub (polysaccharide condensate) surface generate molecular link respectively, with shallow lake
The increase of powder concentration, molecular link quantity increase, and the bonding point of plural gel and contacting substrate increases, therefore adhesion strength increases.With
Unlike the former two, when starch concentration increases to 10wt%, the peeling-off time is obvious between plural gel and contacting substrate
Extend, illustrate before removing occurs, gel has apparent stretching phenomenon, and silica and plural gel and contacting substrate occur
The isolated time is less than 5s.And as shown in Figure 15, adhesion strength between starch plural gel and stainless steel is maximum, this also with first two
Plural gel is different, it is identical be same polytetrafluoroethylene (PTFE) adhesion strength it is all most weak, this illustrates plural gel and contacting substrate
Between adhesion strength in addition to related with the material of contacting substrate, it is also closely bound up with the type and concentration of reinforcing agent particle.
Therefore, in order to study influence of the reinforcing agent particle to adhesion strength, Figure 16, Figure 17 and Figure 18 have been investigated respectively same
Different reinforcing agent plural gels are in contact with it the adhesion strength of generation in matrix.By figure comparison it is found that silica plural gel with
The adhesion strength of three kinds of contacting substrates is maximum, this is consistent with observation when preparing gel rubber system in experiment.Stainless steel is contacted
Matrix, starch plural gel are bigger than the peel adhesion of montmorillonite；And for organic glass contacting substrate, stripping of the latter than the former
It is big from adhesion strength.But the two is close with the adhesion strength of polytetrafluoroethylene (PTFE) matrix.In addition, stainless steel and two kinds of organic glass contacts
Matrix and the adhesion values of compound system are not much different, but the adhesion strength of polytetrafluoroethylene (PTFE) matrix and plural gel is weaker, especially
It is montmorillonite and starch compound system and the adhesion values about 1N of polytetrafluoroethylene (PTFE) or so.This result further illustrates compound solidifying
Adhesion strength between glue and contacting substrate by adhesive (plural gel) be attached matrix and influenced.
Two, the adhesive mechanism between plural gel and contacting substrate is probed into
Adhesion strength is the intermolecular or interatomic active force that two kinds of materials or surface are attached to each other generation.Adhesion process is
One is related to the complicated physics and change of the multiple fields such as rheology, surface chemistry, physical chemistry, polymer physics and chemistry
Process, and adhesiveness power is related with the physical property of the surface nature of contact material and binding itself.Adhesive mechanism
The physical and chemical properties it should be understood that adhesive surface are studied, when two substances of contact are peeling-off, adhesion strength is no longer valid.Mesh
Before a variety of adhesive mechanisms have been proposed explain adhesion strength occur and failure root, but not yet a general theory can
Accurately and reasonably to explain different adhesions.The present invention has studied the adhesion strength between plural gel and different contacting substrates
Difference, it is same multiple although peel adhesion between the two is since different degrees of stretching can occur for the viscoplasticity of plural gel
It is larger to close adhesion strength difference of the gel when the contacting substrate with unlike material separates.For answering under identical particle concentration
It closes for gel, the peel adhesion between plural gel and contact medium is affected by contacting substrate surface nature, therefore
By studying the surface nature of contacting substrate to probe into the adhesive mechanism of plural gel and contacting substrate.
1, mechanical couplings are theoretical
Mechanical couplings theory, which is established, to be had the surface of solids on absolutely rough basis.Pass through scanning electron microscope
(SEM) microstructure of three kinds of stainless steel, organic glass and polytetrafluoroethylene (PTFE) contacting substrate surfaces, such as Figure 19 have been investigated respectively.
It appears from figure 19 that stainless steel surface is in polygon under identical amplification factor, there are many recess and weight not of uniform size
Different cracks；The also out-of-flatness of the surface of organic glass, there are the protrusion of superposition and recess.In contrast, polytetrafluoroethylene (PTFE)
Surface smoother, Cong Tuzhong only observe two or three subtle slight crack.Composite gel system has certain before at adhesive curing
Mobility can be deep into the recess and hole for being glued stromal surface.After gel rubber system solidification, just like countless small
" pin " is tightly embedded in groove or crack, so that mechanically keyed contacts glued touching matrix.Further, since uneven surface
Whole, the presence of recess and crack, there are apparent contact area and real contact areas with the contact of matrix is glued for compound system
Difference.Concave-convex surface degree senior general makes real contact area much larger than apparent contact area, this plural gel and contact surface
Between the good extension being mutually embedded with conducive to contact area, promote the generation of adhesion strength.Figure 19 observes organic glass and not
Become rusty steel the different recess of surface degree and raised range it is larger, both infer accordingly with the degree of adhesion of plural gel compared with
Height, polytetrafluoroethylene (PTFE) then due to surface is smooth and adhesion strength is on the weak side, and this infers and grinds with first part (measurement of adhesion strength)
It is consistent to study carefully result.Therefore composite gel system and the surface adhesion power of contacting substrate and the surface microstructure of the latter are close
Cut phase is closed.
2, surface wetting theory
Adherency results from the intimate contact of two kinds of storerooms, to derive atom or intermolecular work between two interfaces
With.In order to obtain good adsorptivity, the contact distance of the two have to it is small to Van der Waals force or hydrogen bond action can be generated, because
This, the good wetting between interface is most important.In adhesion process, solid, liquid contact surface disappears first, generates new solid-liquid
Interface.If Figure 20 indicates that drop flattens weighing apparatus schematic diagram on solid matrix upper berth, under thermodynamic equilibrium state, according to the side Young
Journey:
γSV=γSL+γLV·cosθ (1)
In formula, θ is contact angle, also referred to as angle of wetting, and contact angle θ is smaller, and wettability is better；γSVFor solid gas interface
Power；γLVFor liquid gas interface tension；γSLFor solid-liquid interfacial tension.
Table 2 lists deionized water on three kinds of stainless steel, organic glass and polytetrafluoroethylene (PTFE) contacting substrate surfaces respectively
Static contact angle numerical value, as seen from table, the contact angle on polytetrafluoroethylene (PTFE) matrix surface are maximum, are 104 °~130 °, and stainless steel
It is respectively 56 °~66 ° and 60 °~76 ° with the contact angular region on organic glass surface.90 ° of the contact angle θ > of stainless steel and water,
Category hates liquid solid；90 ° of the contact angle θ < of stainless steel and organic glass, the two category lyophily solid.Illustrate compared to stainless steel and organic
Glass, water is poor in polytetrafluoroethylene (PTFE) matrix wettability of the surface, composite hydrogel (water content is greater than 90%) and this matrix table
The contact in face is poor, hence it is evident that is weaker than stainless steel and organic glass, therefore composite hydrogel and stainless steel and organic glass connect
It touches tightness and is greater than polytetrafluoroethylene (PTFE).The contact angle for comparing stainless steel and organic glass finds that the former is more slightly smaller than the latter, it was demonstrated that
Water is more slightly higher than organic glass in the wetability of stainless steel surface, illustrates composite hydrogel and the former contact in contrast slightly
By force, but with the latter it is not much different, and first part's (measurement of adhesion strength) also shows plural gel in stainless steel and organic glass
The adhesion strength on surface is close.Power and machinery of the plural gel that wetability mechanism is explained in different contacting substrate surface adhesions
The trend that coupling mechanism illustrates is consistent.
The contact angle of table 2 water and three kinds of matrix
In order to analyze the wetting characteristics of the surface of solids, critical surface tension also is commonly used to characterize.Homologue is measured to same
A kind of contact angle θ of the surface of solids, and by cos θ to surface tension of liquid σLMapping, can obtain a straight line for homologue liquid,
Expression formula is cos θ=a σL+ b, by linear extrapolation to θ=1 cos, available one indicates the numerical value of the surface of solids feature,
Zisman defines the critical surface tension γ that this value is liquid versus solid wettingc, therefore the formula becomes γc=(1-b)/a.?
All surface tension are less than γ in the liquid analogscLiquid, can be spread on the surface of solids with zero degree contact angle.Through
Access learns critical surface tension such as table 3 of three kinds of materials at 20 DEG C, and surface tension of the water at 20 DEG C is 72.75mNm-1, it is smaller than the critical surface tension of stainless steel, therefore water can be sprawled in stainless steel surface, hydrogel is contacted with stainless steel matrix
Well.Although water is bigger than the critical surface tension of polytetrafluoroethylene (PTFE) and organic glass, surface tension is closer to the surface of water
Power, it is opposite with the wetting effect of water better, therefore compare the critical surface tension 18mNm of polytetrafluoroethylene (PTFE)-1, water is in organic glass
More preferably, hydrogel and the contact on organic glass surface are closer for the wetability of glass stromal surface.Therefore it is not added with reinforcing agent grain
The Blank gel of son and the adhesion strength of stainless steel are greater than organic glass, and the latter is greater than polytetrafluoroethylene (PTFE) again, Fig. 7 of this and measurement
Blank gel in (nano silica plural gel), Figure 11 (montmorillonite Composite gel) and Figure 15 (starch plural gel) exists
Adhesion strength trend on three kinds of different contacting substrates is consistent.And shadow of the adhesion strength by particle between plural gel and contacting substrate
It rings, regularity variation is not completely consistent with Blank gel, therefore montmorillonite, silica plural gel and organic glass
Adhesion strength it is higher than stainless steel, the adhesion strength of starch plural gel and stainless steel is higher than organic glass, but unquestionable,
Compared to stainless steel and organic glass, three kinds of plural gels and the adhesion strength of polytetrafluoroethylene (PTFE) matrix are most weak.
The critical surface tension of 3 three kinds of materials of table
Three, adhesion strength/mechanical strength of plural gel and its pressure-resistant sexual intercourse
Plural gel slug is suspended in pit shaft, is played the role of equilibrium strata pressure and is blocked pit shaft so that oil-gas Layer is isolated.
Laboratory utilizes the pressure-resistant performance of pressure resistant testing device analog composite gel slug, if the air pressure of external application is more than plural gel
Voltage endurance capability, plural gel slug will be broken.Since plural gel slug relies on self-strength and and tube wall in casing
Adhesion strength it is jointly pressure-resistant, therefore breakthrough root of plural gel during pressure resistance is strong and weak in the performance with the two performance.This
The relationship of adhesion strength between the pressure-resistant intensity and tube wall with itself of the main research plural gel in part.
Using the pressure-resistant process of organic glass visualization pressure-resistant apparatus measurement plural gel, can be more visible observe is multiple
The different breakthrough modes of gel are closed, as a result as shown in figure 21, in order to illustrate pressure resistance and the relationship of gel mechanical performance and adhesion strength,
The representative breakthrough mode of three formula systems generation, the formula of gel such as table 4 are targetedly selected.
The formula of 4 composite gel system of table
By Figure 21 (a) as it can be seen that 3wt% montmorillonite Composite gel strength is low, nitrogen pressure is weaker from gel body intensity
Center is walked upwards, and gel stress surface integrally presents convex globoidal, when additional nitrogen pressure continues to increase, plural gel because bulk strength compared with
Weak and internal generation, which is bubbled, to be broken through.When reinforcing agent particle concentration increases to 5wt% and 7wt%, plural gel intensity is mentioned
Height, the nitrogen being passed through at this time are no longer fled inside gel, but are elapsed entire gel slug and moved up or between gel and tube wall
Has channeling occurs, causes plural gel to be broken through and pressure resistance failure, such as Figure 21 (b) and Figure 21 (c).Latter two break through mode be because
Caused by plural gel and casing wall adhesion strength are weak.It can thus be appreciated that the pressure-resistant performance of plural gel is not only strong by plural gel ontology
The influence of degree, also adhesion strength is influenced between by gel and casing wall, and the performance value of compressive resistance is its gel body intensity and glues
The attached coefficient result of power.
Table 5 and table 6 are polymer concentration 2wt%, thiourea concentration 0.2wt%, acetic acid chromium concn 0.2wt% and reinforcing agent
(montmorillonite, nano silica) content is respectively the plural gel of 0wt%, 1wt%, 3wt%, 5wt% and 7wt% preparation,
Compressive resistance and breakthrough mode in stainless steel tube, Figure 22 is the adherency with stainless steel matrix respectively of two kinds of system plural gels
The rule that power changes with enhancer concentration.
Analyzed by table 5, table 6 and Figure 22 it is found that with reinforcing agent particle concentration increase, nano silica and montmorillonite
The compressive resistance of plural gel is all gradually increased with the adhesion strength of stainless steel tube wall and mechanical strength.But plural gel pressure resistance
Breakthrough mode is but different with the increase of particle concentration.When montmorillonite concentration is 0wt%~3wt%, nanometer titanium dioxide silicon concentration
When for 0wt%~5wt%, the pressure-resistant breakthrough mode of plural gel is interior bubble, and nitrogen is strong inside plural gel at this time
It spends weaker center to be bubbled, illustrates that the adhesion strength between plural gel and stainless steel tube wall is higher, the caking property of the two is good,
And the mechanical strength of plural gel is the limiting factors of pressure resistance, therefore when particle concentration is low, the mechanical strength of plural gel is
Influence the principal element of compressive resistance.When montmorillonite concentration is between 5wt%~7wt%, nanometer titanium dioxide silicon concentration is in 7wt%
When, plural gel breaks through mode for tube wall breakthrough, and gas is fled between plural gel and tube wall at this time or air pressure pushes
Plural gel is peeling-off with tube wall.According to Figure 22, the adhesion strength of the plural gel under high enhancer concentration is in the trend increased,
But plural gel is because breaking through with the weak generation tube wall of tube wall adhesion strength instead.Although this explanation plural gel mechanical strength with
Adhesion strength enhances with the increase of particle concentration, but compares adhesion strength, and the amplification degree of gel own mechanical intensity is bigger, because
The pressure resistance of this plural gel under the concentration range and stainless steel tube wall has occurred tube wall breakthrough, and the adherency between the two at this time
Power is the short slab of pressure resistance.The breakthrough of such phenomenon also exactly confirm the pressure resistance of plural gel be by gel own mechanical intensity and
The coefficient result of adhesion strength between tube wall.In addition, the pressure resistance of montmorillonite and nano silica plural gel it is most with
Based on interior bubble is broken through, this is all higher related derived from the adhesion strength between two kinds of plural gels and stainless steel tube wall, such as Figure 22.Especially
It is that the adhesion strength of nano silica plural gel is increased to close to 20N, and montmorillonite increases to 7.5N, this also with nanometer in table 6
Breakthrough mode is bubbled in the pressure resistance breakthrough of silica to be consistent more than montmorillonite Composite gel.
Pressure resistance experiment (one) of the 5 montmorillonite Composite gel of table in stainless steel tube
Pressure resistance experiment (two) of the 6 nano silica montmorillonite Composite gel of table in stainless steel tube
The breakthrough pressure and breakthrough of various concentration montmorillonite and nano silica plural gel in polyfluortetraethylene pipe
Mode, such as table 7 and table 8.The rule that two kinds of system plural gels and the adhesion strength of polytetrafluoroethylene (PTFE) matrix change with enhancer concentration
Rule such as Figure 23.
Pressure test (one) of the 7 montmorillonite Composite gel of table in polyfluortetraethylene pipe
Pressure test (two) of the 8 nano silica plural gel of table in polyfluortetraethylene pipe
As shown in Table 7, based on pressure resistance of the plural gel in polyfluortetraethylene pipe is broken through with tube wall, especially montmorillonite
Particle concentration when increasing to 7wt% by 1wt%, based on pressure resistance is broken through with tube wall.And nano silica is in 3wt%-7wt%
Shi Jun is that tube wall breaks through (table 8).This illustrates that the adhesion strength between plural gel and polyfluortetraethylene pipe is very weak.Even if by table 7, table
8 and Figure 23 is it is found that montmorillonite Composite gel and Nano-meter SiO_22The compressive resistance of plural gel and viscous with polytetrafluoroethylene (PTFE) tube wall
Attached power increases with the increase of reinforcing agent particle concentration, but the still majority of the breakthrough between plural gel and tube wall is broken through with tube wall
Based on, this illustrates that the adhesion strength of plural gel and polytetrafluoroethylene (PTFE) tube wall is the principal element for influencing its compressive resistance.
Pressure test (one) of the 9 montmorillonite Composite gel of table in lucite tube
Pressure test (two) of the 10 nano silica plural gel of table in lucite tube
Table 9 and table 10 show the breakthrough pressure of various concentration silica and montmorillonite Composite gel in lucite tube
Power and breakthrough mode, Figure 24 show two kinds of system plural gels and the adhesion strength of organic glass matrix changes with enhancer concentration
Rule.Contrast table 9, table 10 and Figure 24 are it is found that montmorillonite Composite gel and Nano-meter SiO_22The breakthrough pressure of plural gel and with
The adhesion strength of organic glass tube wall increases with the increase of reinforcing agent particle concentration.When reinforcing agent particle concentration is 0wt%
It is to be bubbled that~1wt%, plural gel and tube wall pressure resistance, which break through mode, and nitrogen is not broken through from the engagement edge of gel and tube wall,
That is the adhesion strength of plural gel and organic glass tube wall is enough the tight bond of support gel rubber and tube wall, at this time the machine of plural gel
Tool intensity is to influence the principal element of its compressive resistance.When reinforcing agent particle concentration is in 3wt%~7wt%, pressure-resistant breakthrough side
Formula is tube wall breakthrough, and as adhesion strength increases, breakthrough pressure also increases, it is known that plural gel and organic glass in the concentration range
The adhesion strength of glass tube wall is the principal element for influencing its compressive resistance.In addition, comparison plural gel and three kinds of unlike material tube walls
The number of breakthrough mode compares, the pressure resistance with stainless steel based on being bubbled, based on pressure resistance with polytetrafluoroethylene (PTFE) is broken through with tube wall,
And between with the pressure resistance of organic glass, this is from the plural gel that measures in first part (measurement of adhesion strength) and different materials
The adhesion strength power performance trend of matter tube wall is consistent.
By above-mentioned experimental data can, obtain as drawn a conclusion:
1, peel adhesion is influenced by reinforcing agent particle kind, concentration and contacting substrate material.Peel adhesion and grain
The increase of sub- concentration is proportional to.Compared to montmorillonite and starch, the peel adhesion of nano silica plural gel and matrix
Power is maximum.Compared to polytetrafluoroethylene (PTFE), the adhesion strength of stainless steel and organic glass and compound system is stronger.
2, the mechanical couplings between adhesive mechanism and gel and contacting substrate and wetability are related.Stainless steel and organic glass table
There is recess or crack in face, there is the effect being mutually coupled between compound system and matrix, and the two real contact area is greater than apparent
Contact area；And deionized water and the contact angle of stainless steel and organic glass are smaller than polytetrafluoroethylene (PTFE), hydrogel and the above two
Contact is better than the latter, therefore gel and the adhesion strength of the two are much higher compared with polytetrafluoroethylene (PTFE).
3, the compressive resistance of plural gel is gel mechanical strength and the coefficient result of adhesion strength.Compared between tube wall
Adhesiveness, when plural gel mechanical strength is weak, voltage-withstand test with gel interior bubble breakthrough, therefore work as reinforcing agent particle concentration
Lower (0~1wt%), plural gel are mostly broken through in a manner of interior bubble.After gel mechanical strength itself improves, particle concentration
When higher (7wt%~10wt%), voltage-withstand test is broken through in such a way that has channeling between tube wall or gel integrally move up.When particle is medium dense
When spending (3wt%~5wt%), adhesion strength is influenced by particle types and with tube wall material, therefore compound system breakthrough mode is different.
Claims (3)
1. a kind of measuring device of gel macroscopic adhesion forces, it includes pedestal and upper cover, and the upper cover is covered on the pedestal
Form accommodation space；
It is to be threadedly engaged between the pedestal and the upper cover；
It is set on the side wall of the pedestal there are two opposite watch window, the watch window is set to the opening of the pedestal；
The upper lid is equipped with a through-hole, and a cylinder is hung on the upper lid by the through-hole, and the cylinder is another
End extends to the position corresponding position of the watch window；
The cylinder is hung on the upper lid by the outer that its end is arranged；
The pedestal, the upper cover and the cylinder are in cylindrical；
The material of the pedestal, the upper cover and the cylinder is stainless steel, polytetrafluoroethylene (PTFE) or organic glass；
The upper surface of the cylinder is equipped with a hanged hook or connects a hanged hook by a body of rod；
The internal diameter of the pedestal is 25 ~ 85mm, is highly 30 ~ 80mm；
The diameter and height of the cylinder are 20 ~ 80mm.
2. a kind of gel macroscopic adhesion force measuring system, including the measuring device of gel macroscopic adhesion forces described in claim 1 and
Texture instrument.
3. a kind of gel macroscopic adhesion force measuring method includes the following steps: for gel solution to be placed in gel described in claim 2
In the pedestal of measuring device described in macroscopic adhesion force measuring system, then by the upper cover and the base engagement, make
The upper surface of the gel solution is contacted with the fitting of the lower surface of the cylinder；After the gel plastic, the texture is utilized
Instrument measures the adhesion strength between the gel and the cylinder.
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