CN107703054A - A kind of measurement apparatus and method of gel macroscopic adhesion forces - Google Patents
A kind of measurement apparatus and method of gel macroscopic adhesion forces Download PDFInfo
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- CN107703054A CN107703054A CN201710916930.5A CN201710916930A CN107703054A CN 107703054 A CN107703054 A CN 107703054A CN 201710916930 A CN201710916930 A CN 201710916930A CN 107703054 A CN107703054 A CN 107703054A
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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 a kind of measurement apparatus and method of gel macroscopic adhesion forces.The measurement apparatus includes base and upper lid, and upper be covered on the base forms receiving space；The side wall of the base is provided with two relative watch windows；The upper lid is provided 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 the measurement gel solution that the measurement apparatus of inventive gel macroscopic adhesion forces can quantify contacts plastic with unlike material matrix attachment, the macroscopical peel adhesion occurred between gel and contacting substrate, and the adhesion difference between gel and unlike material contacting substrate can be contrasted, 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 a kind of measurement apparatus and method of gel macroscopic adhesion forces, the adhesion for belonging to high-strength gel is surveyed
Amount field.
Background technology
It is drilled in underbalance in well and uses pressure-resistant technique gel valve, vacantly forming one section in sleeve pipe has mechanical strength
High viscosity gels slug, gel slug using its own mechanical strength and block pit shaft with flat with contacting the adhesiveness of tube wall
Weigh strata pressure, so as to prevent oil gas from revealing, while avoids pollution of the overbalance operation to reservoir caused by drilling well and well killing fluid,
There is isolation, sealing and pressure-bearing, and the pressure-resistant performance for improving gel valve prevents its breakthrough from must just improve the machine of frozen glue
Tool intensity and adhesiveness.The characterizing method of frozen glue mechanical strength is many at present, and the means of the relatively measure adhesiveness of accreditation are to utilize
AFM (AFM) measures microcosmic adhesion (μ N), but not yet finds the method for testing of system and suitable measurement apparatus
Macroscopic adhesion forces are determined, accordingly, it is desirable to provide a kind of device and method for measuring macroscopic adhesion forces.
The content of the invention
It is an object of the invention to provide a kind of measurement apparatus and method of gel macroscopic adhesion forces, macroscopic adhesion forces are fluid
The adhesion that adhesion is peeled off occurs after plastic between contacting substrate, by coordinating with Texture instrument, apparatus of the present invention can be quantified and surveyed
The macroscopic adhesion forces between gel and contacting substrate are measured, the influence factor strong and weak available for gel adhesion is investigated, and can measure solidifying
Glue and the different adhesion differences for contacting material, progress directive function is used to the kill-job of gel valve at the scene.
The measurement apparatus of gel macroscopic adhesion forces provided by the present invention, including base and upper lid, it is described upper to be covered on
Receiving space is formed on the base；
The side wall of the base is provided with two relative watch windows；
The upper lid is provided 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 measurement apparatus of described gel macroscopic adhesion forces, the internal diameter of the base can be 25~85mm, highly can be
30~80mm；
The internal diameter of the upper lid can be 25~85mm, highly can be 25~60mm；
The diameter and height of the cylinder can be 20~80mm.
It is detachably to coordinate between the base and the upper lid in the measurement apparatus of described gel macroscopic adhesion forces,
Concretely screw thread coordinates, and the cylinder that can make to be arranged on the upper lid by screw thread is solidifying with being held in the base
Glue realizes that critical interfaces contact.
In the measurement apparatus of described gel macroscopic adhesion forces, the watch window is located at the opening of the base, leads to
The standoff distance between cylinder described in gel liquid and upper part in the base can be observed and connect by crossing the watch window
The degree of touching.
In the measurement apparatus of described gel macroscopic adhesion forces, the cylinder hangs on institute by the outer of its end set
State on lid, realize that the cylinder is successfully equipped on the upper lid, and the cylinder outer wall realizes that zero rubs with the upper lid inwall
Contact is wiped, and in measurement process, the cylinder carries upwards to be influenceed by the upper lid.
In the measurement apparatus of described gel macroscopic adhesion forces, the watch window is symmetrical set, and ensures the transmission of light,
Being capable of the contact with cylinder bottom of accurate observation liquid level when containing coagulant liquid toward base.
In the measurement apparatus of described gel macroscopic adhesion forces, the base, the upper lid and the cylinder are in cylinder
The bodily form.
The material of the base, the upper lid and the cylinder is stainless steel, polytetrafluoroethylene (PTFE) or lucite etc.；
Wherein, carbon steel material of the stainless steel close to live sleeve pipe；Visual testing can be carried out using lucite tube；It is poly-
Tetrafluoroethene material has high lubrication non-stick, and category hates liquid (water) material；Therefore can be by being glued on above-mentioned three kinds of contacting substrates
The measure of attached property and contrast, and then the adhesiveness of quantitative assessment (compound) gel.
In described gel adhesion force measuring device, the upper surface of the cylinder is provided with a hanged hook or connected by a body of rod
Connect a hanged hook, during measurement, hung up the cylinder by the hanged hook, i.e., by the hanged hook by the cylinder from institute
State and peeled off on gel.
The body of rod can be embedded in the column body by way of screw thread cooperation.
In described gel adhesion force measuring device, the size of the base, the upper lid and the cylinder can be according to need
It is adjusted.
The measurement apparatus of gel macroscopic adhesion forces of the present invention can coordinate with Texture instrument, realize to gel adhesion
Measurement；It can be carried out as steps described below during specific measurement：Gel solution is placed in the measurement apparatus of the gel macroscopic adhesion forces
The base in, then by the upper lid and the base engagement, make the upper surface of the gel solution and the cylinder
Lower surface contact (just contacts)；After the gel plastic, using the Texture instrument measure the gel and the cylinder it
Between adhesion；In measurement process, under the drive of strength sensing member, the column vertical at the uniform velocity moves up, the gel
With the cylinders contact matrix with adhesion caused by the whole process of temporal separation, it is bent that adhesion measurement is obtained by computer record
Line.
The measurement gel solution and unlike material matrix attachment that the measurement apparatus of inventive gel macroscopic adhesion forces can quantify
After contacting plastic, macroscopical peel adhesion for occurring between gel and contacting substrate, and gel can be contrasted and contact base with unlike material
Adhesion difference between matter, this not only oil field underbalance is 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.
Brief description of the drawings
Fig. 1 is the structural representation that inventive gel adheres to force measuring device.
Fig. 2 is that inventive gel adheres to the structural representation that force measuring device coordinates with Texture instrument.
Each mark is as follows in figure：
1 base, lid, 3 watch windows, 4 cylinders, 5 bodies of rod, 6 Texture instruments on 2.
Fig. 3 is that adhesion changes over time curve between silica plural gel and stainless steel in the embodiment of the present invention 2.
Fig. 4 is that adhesion changes over time between 5wt% silica plural gel and stainless steel in the embodiment of the present invention 2
Curve.
Fig. 5 is adhesion between silica plural gel and polytetrafluoroethylene (PTFE) anaplasia at any time in the embodiment of the present invention 2
Change curve.
Fig. 6 be the embodiment of the present invention 2 between 10wt% silica plural gel and lucite adhesion with the time
Change curve.
Adhesion comparison diagrams of the Fig. 7 for silica plural gel in the embodiment of the present invention 2 from different contacting substrates.
Fig. 8 is that the adhesion 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 in the embodiment of the present invention 2 between montmorillonite Composite gel and lucite changes over time song
Line.
Figure 10 is that the adhesion in the embodiment of the present invention 2 between montmorillonite Composite gel and polytetrafluoroethylene (PTFE) changes over time
Curve.
Adhesion comparison diagrams of the Figure 11 for montmorillonite Composite gel in the embodiment of the present invention 2 from different contacting substrates.
Figure 12 is that the adhesion 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 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 in the embodiment of the present invention 2 between the compound solidifying lucite of starch changes over time curve.
Adhesion comparison diagrams of the Figure 15 for starch plural gel in the embodiment of the present invention 2 from different contacting substrates.
Figure 16 is the adhesion comparison diagram of different composite gel and stainless steel contacting substrate in the embodiment of the present invention 2.
Figure 17 is the adhesion comparison diagram of different composite gel and lucite contacting substrate in the embodiment of the present invention 2.
Figure 18 is the adhesion 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 lucite；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) moves up to be overall, Figure 21
(c) broken through between tube wall.
Figure 22 is the adhesion between different composite gel and stainless steel rotor (cylinder) in the embodiment of the present invention 2.
Figure 23 is the adhesion between different composite gel and polytetrafluoroethylene (PTFE) rotor (cylinder) in the embodiment of the present invention 2
Power.
Figure 24 is the adhesion between different composite gel and lucite rotor (cylinder) in the embodiment of the present invention 2.
Embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
Material used, reagent etc., unless otherwise specified, are commercially obtained in following embodiments.
Embodiment 1, gel adhesion force measuring device
As shown in figure 1, the structural representation of the measurement apparatus for inventive gel macroscopic adhesion forces, it includes the He of base 1
Upper lid 2, base 1 and upper lid 2 are in cylindrical, and base 1 can be matched somebody with somebody by screw thread with upper lid 2 and merge to form receiving space.Its
In, the internal diameter of base 1 is 60mm, is highly 50mm, and the internal diameter of upper lid 2 is 60mm, is highly 35mm.Set in the side wall of base 1
There are 2 symmetrical watch windows 3, and watch window 3 is located at the opening of base 1.Upper lid 2 is provided with a manhole (figure
In do not mark), a cylinder 4 is hung on upper lid 2 by manhole, and the other end of cylinder 4 extends to watch window 3
Position corresponding position, i.e., the bottom of cylinder 4 is able to observe that by watch window 3, the diameter and height of cylinder 4 are
50mm.In the present invention, the outer (not marked in figure) that cylinder 5 is set by upper end is hung on upper lid 2.The interior edge of cylinder 4
It is axially arranged with a body of rod 5, and by way of screw thread cooperation in cylinder 4, the free-end of the body of rod 5 is provided with to be hanged the body of rod 5
Hook.
In inventive gel adhesion force measuring device, the size of base 1, upper lid 2 and cylinder 4 can be adjusted as needed
It is whole.
In the measurement apparatus of inventive gel macroscopic adhesion forces, the material of base 1, upper lid 2 and cylinder 4 may be selected stainless
Steel, polytetrafluoroethylene (PTFE) or lucite etc., wherein, carbon steel material of the stainless steel close to live sleeve pipe；Using lucite tube
Visual testing can be carried out；Polytetrafluoroethylene (PTFE) material has high lubrication non-stick, and category hates liquid (water) material；Therefore can be by upper
State the measure of adhesiveness and contrast on three kinds of contacting substrates, and then the adhesiveness of quantitative assessment (compound) gel.
As shown in Fig. 2 the measurement apparatus of inventive gel macroscopic adhesion forces can be coordinated with Texture instrument 6, realization pair
The measurement of gel adhesion.It can be carried out as steps described below during specific measurement：Gel solution is placed in gel adhesion measurement dress
In the base 1 put, then upper lid 2 is coordinated with base 1, the upper surface of gel is contacted with the lower surface of cylinder 4 and (just connects
Touch)；After gel plastic, the adhesion between gel and cylinder 4 is measured using Texture instrument 2；In measurement process, in strength sense
Under Ying Yuan drive, cylinder 4 vertically at the uniform velocity moves up, whole mistake of the gel with the contacting substrate of cylinder 5 with temporal separation
Adhesion caused by journey, adhesion experiment curv is obtained by computer record.
The application of embodiment 2, gel adhesion force measuring device
First, between plural gel and contacting substrate adhesion quantitative determination
About 100g plural gels are taken to pour into the base 1 of the measurement apparatus of the gel macroscopic adhesion forces of embodiment 1.It will carry
The upper lid 2 of cylinder 4 is slowly contacted by the rotation of screw thread with the part of base 1, passes through the watch window 3 in the side wall of base 1
Observation coagulant liquid just contacts with the cylinder 4 of upper part, measures whole gel adhesion with adhesive tape and preservative film and fills
Sealing is put, is placed in 70 DEG C of thermostatic drying chambers and reacts, is taken out after being crosslinked 24h, adhesive tape and preservative film is removed, is connected with Texture instrument
The plural gel is measured with contacting the adhesion between rotor (cylinder 4).
Adhesion quantitative determination in, composite gel system by 2wt% polyacrylamides, 0.2wt% chromium acetates,
0.2wt% thiocarbamide and concentration is respectively that 0wt%, 1wt%, 3wt%, 5wt%, 7wt% and 10wt% reinforcing agent (cover de-
Soil, silica and starch) composition, formula is as shown in table 1, and this formula takes out measurement at 70 DEG C after plastic 24h.
The formula of the composite gel system of table 1
1st, the adhesion of silica plural gel
The adhesion of silica plural gel and stainless steel contacting substrate changes over time curve such as Fig. 3, and adhesion 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
Cylinder top half when at the uniform velocity being lifted upwards in the presence of Texture instrument tension belt, the stainless steel cylinder that is adhered to each other originally
Tear and separate with plural gel, strength sensing member senses gel that cylinder is subject to its downward adhesion, with drawing
The increase of distance is stretched, this power gradually increases；The stainless steel cylinder of second stage (b), plural gel and adhesion contact is peeling-off
Moment, now strength sensing member senses cylinder by the downward maximum adhesion power of 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 for the latter that the former is subject to is less and less, 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 has significant impact.With the increase of silica concentration, the adhesion between plural gel and stainless steel contact surface
Power shows a rising trend.This is relevant with the molecular force of stainless steel stromal surface with nano silicon.Stainless steel surfaces are due to Fe-OH
With the distribution presence-OH groups of iron oxide, and there are three kinds of different bond styles in the big nano-silica surface of specific surface area
Hydroxyl, be single raw silicone hydroxyl, adhesion association silicone hydroxyl and twin silicone hydroxyl respectively, when nano silicon plural gel with not
During steel surface of becoming rusty contact, except polymer chain, the active force of water and stainless steel surfaces, nano-silicon dioxide particle and stainless steel watch
- the OH in face forms intermolecular hydrogen bonding, and nano-silicon dioxide particle concentration is higher, and its hydrogen bond quantity contacted with stainless steel surfaces carries
The caking property of height, plural gel and stainless steel surfaces is strengthened, therefore the adhesion between the two is with nano silicon ion concentration
Increase and increase.
Fig. 5 and Fig. 6 is respectively the adhesion experiment curv between plural gel and polytetrafluoroethylene (PTFE), lucite.Can by figure
Know, with the increase of silica concentration, the adhesion between plural gel and contacting substrate is gradually increasing, except that adhesion
The difference of power.The maximum of adhesion between plural gel and contacting substrate under various concentrations, i.e. peak value in Fig. 2 curves are taken respectively
B, the weight with the matrix rotor of gel contacts is individually subtracted, obtains the adhesion 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 more or less the same, but when particle concentration increases to 10wt% from 5wt%, the peel adhesion between lucite
Power is respectively 23.839N, 25.184N and 40.930N, and the adhesion between stainless steel is respectively 19.998N, 22.521N and
33.066N, the adhesion between plural gel and lucite are slightly larger than stainless steel.
2nd, the adhesion of montmorillonite Composite gel
Fig. 8-Figure 11 is respectively between montmorillonite Composite gel and stainless steel, lucite and polytetrafluoroethylene (PTFE) contacting substrate
Separate adhesion test curve.As seen from the figure with the increase of particle concentration, between plural gel and stainless steel and lucite
Separation adhesion gradually increases, and the adhesion change between polytetrafluoroethylene (PTFE) is little.Because the piece layer architecture surface tool of montmorillonite
Have a number of hydroxyl, and surface is negatively charged, when being contacted with stromal surface, respectively with the-OH of stainless steel surfaces, organic glass
- C-O and the O-C=O group on glass (polymethyl methacrylate) surface produce molecular link, with the increase of particle concentration, molecule
The bonding point intensity increase of the increasing number of key, plural gel and stromal surface.Polytetrafluoroethylene (PTFE) is the nonpolar of high degree of symmetry
High polymer material, there is excellent heat endurance, faint dispersion force between montmorillonite be present, therefore with montmorillonite concentration
Increase, the adhesion amplitude of variation between plural gel and polytetrafluoroethylene (PTFE) are smaller.
Contrast adhesion between low concentration and high concentration montmorillonite Composite gel and contacting substrate and peel off curve discovery, in montmorillonite
During 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 stripping is higher than 70s, and 1wt% montmorillonite Composite gels are 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 Composites gel and contacting substrate
Peel off and occur within 5s.In influence of fourth, fifth, the six chapters research reinforcing agent particle to performance, it has been found that plural gel glues
Elasticity increases with the increase of particle concentration, and plural gel is generally accompanied by during being separated with contacting substrate and coagulated
The draw stage of glue, after gel stretching to a certain extent, adhesion occurs with contacting substrate and separates.Therefore deduce 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.Reason be for the plural gel under low concentration (≤3wt%),
The larger mobility of system and morphotropism support its contact relatively good with stromal surface, cause tight between gel and contacting substrate
Close adhesion, and the elasticity of plural gel body is weaker, therefore gel is incited somebody to action by when the stretching of contact cylinder adhered to it
The elastic stretching of one section of long period first occurs, after elastic stretching is big to a certain extent afterwards, gel just occurs with contacting substrate
Peel off.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 in itself, the adhesiveness of itself and contacting substrate be easier it is first peeling-off, therefore high concentration plural gel by
To the contact cylinder adhered to it stretching when, elastic stretching by a small margin occurs for body 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 lucite matrix is maximum, 35.701N is reached as high as, next to that the adhesion with stainless steel contacting substrate
Peel adhesion of the peel adhesion of power, 10wt% montmorillonite Composites gel and stainless steel between 10.335N, with polytetrafluoroethylene (PTFE)
Power is minimum, and influence of the increase of particle concentration to its adhesion is smaller.Illustrate the composition of contacting substrate to plural gel
Adhesion influences very big.
3rd, the adhesion of starch plural gel
Figure 12-Figure 15 is that the adhesion of starch plural gel contacting substrate different from three kinds peels off experiment curv.Can by figure
Know, with the increase of starch concentration, the adhesion between plural gel and stainless steel and lucite gradually increases, with polytetrafluoro
Adhesion between ethene has almost no change.This is similar with the enhancing trend of silica and montmorillonite particle.Due to amylum body
Hydroxyl-the OH and the group on stainless steel and lucite surface on sub (polysaccharide condensate) surface produce molecular link respectively, with shallow lake
The bonding point of the increase of powder concentration, molecular link increasing number, plural gel and contacting substrate increases, therefore adhesion 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 generation is peeled off, gel has obvious stretching phenomenon, and silica and plural gel occur with contacting substrate
The time of separation is less than 5s.And as shown in Figure 15, adhesion between starch plural gel and stainless steel is maximum, this also with first two
Plural gel is different, and identical is that the adhesion of same polytetrafluoroethylene (PTFE) is all most weak, this explanation plural gel and contacting substrate
Between adhesion except relevant 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, Figure 16, Figure 17 and Figure 18 have investigated same respectively
Different reinforcing agent plural gels are in contact with it caused adhesion in matrix.From figure contrast, silica plural gel and
The adhesion of three kinds of contacting substrates is maximum, and this is consistent with observation when gel rubber system is prepared in experiment.Contacted for stainless steel
Matrix, starch plural gel are bigger than the peel adhesion of montmorillonite；And for lucite contacting substrate, stripping of the latter than the former
It is big from adhesion.But the adhesion of the two and polytetrafluoroethylene (PTFE) matrix is close.In addition, two kinds of contacts of stainless steel and lucite
Matrix and the adhesion values of compound system are more or less the same, but the adhesion of polytetrafluoroethylene (PTFE) matrix and plural gel is weaker, especially
It is montmorillonite and the adhesion values of starch compound system and polytetrafluoroethylene (PTFE) about 1N or so.This result further illustrates compound solidifying
Adhesion between glue and contacting substrate is influenceed by adhesive (plural gel) with being attached matrix.
2nd, the adhesive mechanism between plural gel and contacting substrate is probed into
Adhesion is that two kinds of materials or surface are attached to each other caused intermolecular or interatomic active force.Adhesion process is
The one complicated physics for being related to the multiple fields such as rheology, surface chemistry, physical chemistry, polymer physics and chemistry and change
Process, and the strong and weak physical property with the surface nature and binding of contact material of adhesiveness in itself is relevant.Adhesive mechanism
Research is it should be understood that the physical and chemical properties of adhesive surface, when two materials of contact are peeling-off, adhesion has failed.Mesh
Before a variety of adhesive mechanisms have been proposed explain adhesion occur and failure root, can but go back neither one general theory
To explain accurately and reasonably different adhesions.The present invention have studied the adhesion between plural gel and different contacting substrates
Difference, it is same multiple although peel adhesion between the two is because different degrees of stretching can occur for the viscoplasticity of plural gel
It is larger to close adhesion difference of the gel when the contacting substrate with unlike material separates.For answering under identical particle concentration
Close for gel, the peel adhesion between plural gel and contact medium is had a great influence by contacting substrate surface nature, therefore
The adhesive mechanism of plural gel and contacting substrate is probed into by studying the surface nature of contacting substrate.
1st, mechanical couplings are theoretical
Theoretical establish of mechanical couplings is present to the surface of solids on definitely rough basis.Pass through ESEM
(SEM) stainless steel, the microstructure on three kinds of contacting substrate surfaces of lucite and polytetrafluoroethylene (PTFE), such as Figure 19 have been investigated respectively.
It appears from figure 19 that under identical multiplication factor, stainless steel surfaces are in polygon, many depressions and weight not of uniform size be present
Different cracks；The also out-of-flatness of the surface of lucite, the projection and depression of superposition be present.Under contrast, polytetrafluoroethylene (PTFE)
Surface smoother, two or three trickle slight crack is only observed from figure.Composite gel system is certain into having before adhesive curing
Mobility, it can be deep into by the depression and hole of viscous stromal surface.After gel rubber system solidifies, just just as countless small
" pin " is tightly embedded in groove or crack, so as to which mechanically keyed contacts glued tactile matrix.Further, since uneven surface
Whole, there is apparent contact area and real contact area in the presence in depression and crack, compound system with by the contact of viscous matrix
Difference.Concave-convex surface degree senior general causes real contact area to be much larger than apparent contact area, this plural gel and contact surface
Between the good extension being mutually embedded with beneficial to contact area, promote the generation of adhesion.Figure 19 observes lucite and not
The depression that differs of surface degree and raised scope of rust steel are larger, infer accordingly both degree of adhesion with plural gel compared with
Height, polytetrafluoroethylene (PTFE) then due to surface is smooth and adhesion is on the weak side, and this infers and ground with Part I (measure of adhesion)
It is consistent to study carefully result.Therefore the surface adhesion of composite gel system and contacting substrate is strong and weak close with the surface microstructure of the latter
Cut is closed.
2nd, surface wetting theory
Adhesion results from the intimate contact of two kinds of storerooms, so as to derive atom or intermolecular work between two interfaces
With.In order to obtain good adsorptivity, both contact distances have to it is small to Van der Waals force or hydrogen bond action can be produced, because
This, the good wetting between interface is most important.In adhesion process, solid, liquid contact surface disappears first, generates new solid-liquid
Interface.As Figure 20 represent drop solid matrix upper berth flatten weighing apparatus schematic diagram, under thermodynamic equilibrium state, according to Young side
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 force；γSLFor solid-liquid interfacial tension.
Table 2 lists deionized water on three kinds of stainless steel, lucite 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 lucite 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 lucite, 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 aquogel (water content is more than 90%) and this matrix table
The contact in face is poor, hence it is evident that is weaker than stainless steel and lucite, therefore composite aquogel and stainless steel and lucite connect
Touch tight ness rating and be more than polytetrafluoroethylene (PTFE).The contact angle for contrasting stainless steel and lucite finds that the former is more slightly smaller than the latter, it was demonstrated that
Water is more slightly higher than lucite in the wetability of stainless steel surfaces, illustrates composite aquogel and the former contact comparatively slightly
By force, but with the latter it is more or less the same, and Part I (measurement of adhesion) displays that plural gel in stainless steel and lucite
The adhesion on surface approaches.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 the water of table 2 and three kinds of matrix
In order to analyze the wetting characteristics of the surface of solids, also characterized through conventional critical surface tension.Homologue is determined to same
A kind of contact angle θ of the surface of solids, and by cos θ to surface tension of liquid σLMapping, a straight line can be obtained for homologue liquid,
Expression formula is cos θ=a σL+ b, by linear extrapolation to cos θ=1, the numerical value for representing the surface of solids feature is can obtain,
Zisman defines the critical surface tension γ that this value is liquid versus solid wettingc, therefore the formula is changed into γc=(1-b)/a.
Every surface tension is less than γ in the liquid analogscLiquid, can be spread over zero degree contact angle on the surface of solids.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 surfaces, hydrogel contacts with stainless steel matrix
Well.Although water is bigger than the critical surface tension of polytetrafluoroethylene (PTFE) and lucite, surface tension is closer to the surface of water
Power, it is relative with the wetting effect of water better, therefore compared to the critical surface tension 18mNm of polytetrafluoroethylene (PTFE)-1, water is in organic glass
More preferably, hydrogel and the contact on lucite surface are closer for the wetability of glass stromal surface.Therefore it is not added with reinforcing agent grain
The Blank gel and the adhesion of stainless steel of son are more than lucite, and the latter is more than polytetrafluoroethylene (PTFE) again, this Fig. 7 with measurement
Blank gel in (nano silicon plural gel), Figure 11 (montmorillonite Composite gel) and Figure 15 (starch plural gel) exists
Adhesion trend on three kinds of different contacting substrates is consistent.And shadow of the adhesion by particle between plural gel and contacting substrate
Ring, its regularity change is not completely consistent with Blank gel, therefore montmorillonite, silica plural gel and lucite
Adhesion it is higher than stainless steel, the adhesion of starch plural gel and stainless steel is higher than lucite, but unquestionable,
Compared to stainless steel and lucite, three kinds of plural gels and the adhesion of polytetrafluoroethylene (PTFE) matrix are most weak.
The critical surface tension of 3 three kinds of materials of table
3rd, adhesion/mechanical strength of plural gel and its pressure-resistant sexual intercourse
Plural gel slug is suspended in pit shaft, plays a part of equilibrium strata pressure closure pit shaft to isolate oil-gas Layer.
Laboratory utilizes the pressure-resistant performance of pressure resistant testing device analog composite gel slug, if the air pressure of external application exceedes plural gel
Voltage endurance capability, plural gel slug will be broken.Because plural gel slug relies on self-strength and and tube wall in sleeve pipe
Adhesion it is jointly pressure-resistant, therefore breakthrough root of the plural gel during pressure-resistant is strong and weak in the performance with the two performance.This
The relation of adhesion between the pressure-resistant intensity and tube wall with itself of the main research plural gel in part.
Using the pressure-resistant process of lucite visualization pressure-resistant apparatus measure plural gel, can be observed again with more visible
The different breakthrough modes of gel are closed, as a result as shown in figure 21, in order to illustrate the relation of pressure-resistant and gel mechanical performance and adhesion,
It targetedly have selected the representational breakthrough mode that three formula systems occur, the formula such as table 4 of gel.
The formula of the composite gel system of table 4
From Figure 21 (a), 3wt% montmorillonite Composite gel strengths are low, and nitrogen pressure is weaker from gel bulk strength
Center is walked upwards, and gel stress surface integrally presents convex globoidal, when additional nitrogen pressure continues increase, plural gel because bulk strength compared with
Weak and internal generation bubbling is broken through.When reinforcing agent particle concentration increases to 5wt% and 7wt%, plural gel intensity is carried
Height, the nitrogen being now passed through no longer are fled inside gel, but are elapsed whole gel slug and moved up or between gel and tube wall
Generation has channeling, plural gel is caused to be broken through and pressure-resistant failure, such as Figure 21 (b) and Figure 21 (c).Latter two break through mode be because
Plural gel is weak caused with casing wall adhesion.It can thus be appreciated that the pressure-resistant performance of plural gel is not only strong by plural gel body
The influence of degree, also adhesion is influenceed between by gel and casing wall, and the performance value of compressive resistance is its gel bulk strength and glued
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 silicon) content is respectively plural gel prepared by 0wt%, 1wt%, 3wt%, 5wt% and 7wt%,
Compressive resistance and breakthrough mode in stainless steel tube, Figure 22 is the adhesion with stainless steel matrix respectively of two kinds of system plural gels
The rule that power changes with enhancer concentration.
Analyzed from table 5, table 6 and Figure 22, with the increase of reinforcing agent particle concentration, nano silicon and montmorillonite
The compressive resistance of plural gel, all gradually increase with the adhesion of stainless steel tube wall and mechanical strength.But plural gel is pressure-resistant
Breakthrough mode is but different with the increase of particle concentration.When montmorillonite concentration is 0wt%~3wt%, nanometer titanium dioxide silicon concentration
For 0wt%~5wt% when, the pressure-resistant breakthrough mode of plural gel is interior bubble, and now nitrogen is strong inside the plural gel
The weaker center bubbling of degree, illustrates that the adhesion between plural gel and stainless steel tube wall is higher, and the caking property of the two is good,
And the mechanical strength of plural gel is pressure-resistant limiting factors, 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 is broken through mode and broken through for tube wall, and now gas is fled between plural gel and tube wall, or air pressure promotes
Plural gel is peeling-off with tube wall.According to Figure 22, the adhesion of the plural gel under high enhancer concentration is in the trend of increase,
But plural gel is because being broken through with the weak tube wall that occurs of tube wall adhesion on the contrary.Although this explanation plural gel mechanical strength with
Adhesion strengthens with the increase of particle concentration, but compares adhesion, and the amplification degree of gel its own mechanical intensity is bigger, because
This plural gel under the concentration range is pressure-resistant there occurs tube wall breakthroughs with stainless steel tube wall, and now both between adhesion
Power is pressure-resistant short slab.The breakthrough of such a phenomenon also exactly confirm plural gel it is pressure-resistant be by gel its own mechanical intensity and
The coefficient result of adhesion between tube wall.In addition, montmorillonite and nano silicon plural gel it is pressure-resistant it is most with
Based on interior bubble is broken through, the adhesion that this is come between two kinds of plural gels and stainless steel tube wall is all higher relevant, such as Figure 22.Especially
It is that the adhesion of nano silicon plural gel is increased to close to 20N, and montmorillonite increases to 7.5N, this also with nanometer in table 6
Bubbling is broken through mode and is consistent more than montmorillonite Composite gel in the pressure-resistant breakthrough of silica.
Pressure-resistant experiment (one) of the montmorillonite Composite gel of table 5 in stainless steel tube
Pressure-resistant experiment (two) of the nano silicon montmorillonite Composite gel of table 6 in stainless steel tube
The breakthrough pressure and breakthrough of various concentrations montmorillonite and nano silicon 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 of polytetrafluoroethylene (PTFE) matrix change with enhancer concentration
Rule such as Figure 23.
Pressure test (one) of the montmorillonite Composite gel of table 7 in polyfluortetraethylene pipe
Pressure test (two) of the nano silicon plural gel of table 8 in polyfluortetraethylene pipe
As shown in Table 7, based on pressure-resistant in polyfluortetraethylene pipe of plural gel is broken through with tube wall, especially montmorillonite
Particle concentration when increasing to 7wt% by 1wt%, it is pressure-resistant broken through with tube wall based on.And nano silicon is in 3wt%-7wt%
Shi Jun is that tube wall breaks through (table 8).Adhesion between this explanation plural gel and polyfluortetraethylene pipe is very weak.Even if by table 7, table
Knowable to 8 and Figure 23, 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, the adhesion of this explanation plural gel and polytetrafluoroethylene (PTFE) tube wall is the principal element for influenceing its compressive resistance.
Pressure test (one) of the montmorillonite Composite gel of table 9 in lucite tube
Pressure test (two) of the nano silicon plural gel of table 10 in lucite tube
Table 9 and table 10 show the breakthrough pressure of various concentrations silica and montmorillonite Composite gel in lucite tube
Power and breakthrough mode, Figure 24 show two kinds of system plural gels and the adhesion of lucite matrix changes with enhancer concentration
Rule.Knowable to contrast table 9, table 10 and Figure 24, montmorillonite Composite gel and Nano-meter SiO_22The breakthrough pressure of plural gel and with
The adhesion of lucite tube wall increases with the increase of reinforcing agent particle concentration.When reinforcing agent particle concentration is 0wt%
~1wt%, plural gel are bubbling with the pressure-resistant breakthrough mode of tube wall, and nitrogen is not broken through from the engagement edge of gel and tube wall,
That is the adhesion of plural gel and lucite tube wall is enough the machine of the tight bond, now plural gel of support gel rubber and tube wall
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 breaks through for tube wall, and as adhesion increases, breakthrough pressure also increases, it is known that plural gel and organic glass in the concentration range
The adhesion of glass tube wall is the principal element for influenceing its compressive resistance.In addition, contrast plural gel and three kinds of unlike material tube walls
The number contrast of breakthrough mode, it is pressure-resistant based on bubbling with stainless steel, with polytetrafluoroethylene (PTFE) it is pressure-resistant broken through with tube wall based on,
And with lucite it is pressure-resistant between, this and the plural gel that is measured in Part I (measurement of adhesion) and different materials
The adhesion power performance trend of matter tube wall is consistent.
By above-mentioned experimental data can, obtain as drawn a conclusion：
1st, peel adhesion is influenceed by reinforcing agent particle kind, concentration and contacting substrate material.Peel adhesion and grain
The proportional relation of increase of sub- concentration.Compared to montmorillonite and starch, the peel adhesion of nano silicon plural gel and matrix
Power is maximum.Compared to polytetrafluoroethylene (PTFE), stainless steel and the adhesion of lucite and compound system are stronger.
2nd, the mechanical couplings between adhesive mechanism and gel and contacting substrate and wetability are relevant.Stainless steel and lucite table
There is depression or crack in face, the effect being mutually coupled between compound system and matrix be present, and the two real contact area is more than apparent
Contact area；And deionized water and the contact angle of stainless steel and lucite ratio polytetrafluoroethylene (PTFE) are small, hydrogel with the above two
Contact is better than the latter, therefore gel and the adhesion of the two are much higher compared with polytetrafluoroethylene (PTFE).
3rd, the compressive resistance of plural gel is gel mechanical strength and the coefficient result of adhesion.Compared between tube wall
Adhesiveness, when plural gel mechanical strength is weak, voltage-withstand test is broken through with gel interior bubble, therefore works as reinforcing agent particle concentration
Relatively low (0~1wt%), plural gel is more to be broken through in a manner of interior bubble.After gel mechanical strength itself improves, particle concentration
When higher (7wt%~10wt%), voltage-withstand test has channeling or gel between tube wall integrally move up in a manner of break through.When particle is medium dense
When spending (3wt%~5wt%), adhesion is influenceed by particle types and with tube wall material, therefore compound system is broken through mode and differed.
Claims (9)
1. a kind of measurement apparatus of gel macroscopic adhesion forces, it includes base and upper lid, described upper to be covered on the base
Form receiving space；
The side wall of the base is provided with two relative watch windows；
The upper lid is provided 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.
2. the measurement apparatus of gel macroscopic adhesion forces according to claim 1, it is characterised in that：The base with it is described on
It is detachably to coordinate between lid.
3. the measurement apparatus of gel macroscopic adhesion forces according to claim 2, it is characterised in that：The base with it is described on
Coordinate between lid for screw thread.
4. the measurement apparatus of the gel macroscopic adhesion forces according to any one of claim 1-3, it is characterised in that：The sight
Examine the opening that window is located at the base.
5. the measurement apparatus of the gel macroscopic adhesion forces according to any one of claim 1-4, it is characterised in that：The post
Body is hung on the upper lid by the outer of its end set.
6. the measurement apparatus of the gel macroscopic adhesion forces according to any one of claim 1-5, it is characterised in that：The bottom
Seat, the upper lid and the cylinder are in cylindrical；
The material of the base, the upper lid and the cylinder is stainless steel, polytetrafluoroethylene (PTFE) or lucite.
7. the measurement apparatus of the gel macroscopic adhesion forces according to any one of claim 1-6, it is characterised in that：The post
The upper surface of body is provided with a hanged hook or connects a hanged hook by a body of rod.
8. a kind of gel adhesion force measuring system, include the measurement of gel macroscopic adhesion forces any one of claim 1-7
Device and Texture instrument.
9. a kind of gel macroscopic adhesion force measuring method, comprises the following steps：Gel solution is placed in any in claim 1-7
In the base of the measurement apparatus of the item gel macroscopic adhesion forces, then by the upper lid and the base engagement, make institute
The upper surface of gel solution is stated to contact with the lower surface fitting of the cylinder；After the gel plastic, the Texture instrument is utilized
Measure the adhesion between the gel and the cylinder.
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