CN108548775A - Enamel coating electrode and preparation method, corrosion resistance test method - Google Patents
Enamel coating electrode and preparation method, corrosion resistance test method Download PDFInfo
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Abstract
The invention belongs to electrochemical material technical fields, and in particular to enamel coating electrode and preparation method, corrosion resistance test method.The technical problem to be solved by the present invention is to measure the corrosion resistance of enamel coating, it is measured by electrochemical methods.The method comprises the steps of firstly, preparing enamel coating electrodes, then the polarization curve with enamel coating electrode, platinum electrode, calomel reference electrode, electrochemical analyser connecting test enamel coating in etchant solution system, calculate the corrosion potential E of enamel coatingcorrWith corrosion electric current density icorr, finally obtain the corrosion rate V of enamel coating.The method of the present invention have many advantages, such as it is easy to operate, take it is short, result is more acurrate.
Description
Technical field
The invention belongs to electrochemical material technical fields, and in particular to enamel coating electrode and preparation method, corrosion resistance
Test method.
Background technology
Enamel coating is a kind of inorganic ceramic glaze of the blackening on metal bottom base surface, has good metal wellability and parent
And power, when firing, enamel forms oxide buffer layer with metal surface, is integrated with metal surface melting.Ceramic glaze surface can prevent
Corrosion of the metal in various systems plays a buffer protection function, reduces the corrosion of metallic matrix.Therefore, enamelware
The performance of the intensity and the magnificent appearance and resistance to chemical attack of enamel of metal is had both.
Currently, the corrosion resistance evaluation of enamel coating is mainly with hot acid liquid or the leaching corruption of 100g/L citric acid solutions of boiling
Evaluate the corrosion resistance of enamel coating.
In the assay method of the resistance to boiling hcl corrosion performance of GB/T7989-2003 enamel for glassed steel, with enamel test specimen through quality
Score 20% boiling hcl corrosion 168h or 336h, measure test specimen mass loss, calculate the matter on unit area in certain time
Amount loss rate, i.e. corrosion rate.Corrosion rate is lower, and enamel for glassed steel is to boiling hydrochloric acid corrosion resisting property better.However this test
The method time is veryer long, and test result error is larger, while can use the waste of a large amount of human and material resources.
In the GB/T9989-2005 enamel citric acid of resistance to room temperature erosion test method, warded off with the erosion of 100g/L citric acid solutions
A part of surface of porcelain coating sample, this method carry out erosion resisting according to the state and cleanable degree on enamel coating surface
Evaluation.A few drop 100g/L citric acid solutions are specially dripped on every piece of sample, are used in combination filter paper to cover, are ensured on enamel coating surface
There are one the treatment regions of continuous Adsorption of Filter Paper citric acid, and diameter should be less than the surface of monoblock enamel coating, with surface ware lid
Firmly citric acid treatment area keeps the temperature of 3 DEG C of 23 scholar to remove surface plate lid after 15min scholar 30s during entire experiment
And citric acid filter paper is blotted with distilled water, deionized water or originally water wash enamel coating specimen surface with new dry filter paper,
It is drawn with pencil and connects subparallel lines through peracid treatment region and untreated area, at highlight from different angles visual acid
The difference for managing area and untreated area, the deciding grade and level of enamel coating corrosion resistance in 100g/L citric acid solutions is judged with this.So
And this test method is fairly simple, can only carry out simple qualitative test, cannot quantify to test out enamel coating corrosion-resistant
The specific data of performance.
Invention content
For defect existing for existing detection enamel coating corrosion resistance, the present invention provides one kind take it is short, simpler,
The test method of more accurate enamel coating corrosion resistance.
Electrochemical corrosion is a special galvano-cautery, i.e., corrodes caused by extrinsic current.Potential polarization curve Tafel is to comment
The index of valence sample corrosion resisting property at room temperature immerses sample in etchant solution system, carries out polarization curve test.Polarization curve
Middle cathode portion is related to the precipitation of hydrogen, and anode part is related to the corrosive nature of sample.Anodic polarization curves refer to from
Corrosion potential starts, and with certain sweep speed, polarization working electrode to a certain selection of appointed obtains current potential and current density
Relation curve.With shuffling for current potential, current density is bigger, then corrosion resistance is weaker, on the contrary then stronger.Therefore, present invention profit
It is evaluated with electrochemical corrosion to test resistance to chemical attack ability, corrosion speed monitor and the inhibition of enamel coating.
First, first technical problem to be solved by this invention is to provide a kind of preparation method of enamel coating electrode.
The preparation method includes the following steps：
A, conducting wire is welded to the metal base surface of enamel coating, then put it into container；
B, epoxy resin and curing agent mixing are removed into bubble removing, add plasticizer mixing and obtain mixture, by mixture plus
Enter in the container of step a and is sealed other faces in addition to enamel coating face；
C, the bubble in the mixture that removal is added to the container, waits for epoxy resin cure, obtains enamel coating electrode.
Specifically, in the preparation method step a of above-mentioned enamel coating electrode, the enamel coating is cut, is ground, clearly
Wash, dry after welded again.
Further, in the preparation method step a of above-mentioned enamel coating electrode, the rotating speed of the cutting is 2800~
3000r/min.The equipment used is cut as Metallographic Specimen Cutting Machine.
Further, in the preparation method step a of above-mentioned enamel coating electrode, it is described grind the sand paper that uses for 240~
700CWAl2O3, rotating speed is 400~500r/min.The equipment used is ground as metallographical polishing machine.Sample is in 90 ° with sand paper face.
Further, it in the preparation method step a of above-mentioned enamel coating electrode, polishes before grinding.The polishing
Rotating speed is 1200~1500r/min, and sample edge is in 70~80 ° of angles with wheel face.The equipment used polish as abrasive machine.Often
3~5s is water-cooled.
Further, in the preparation method step a of above-mentioned enamel coating electrode, the cleaning is first to wash, then use acetone
Or absolute ethyl alcohol is washed.
Specifically, in the preparation method step a of above-mentioned enamel coating electrode, the enamel coating metallic matrix is the length of side
The square or rectangular of 10mm~15mm.
Specifically, in the preparation method step a of above-mentioned enamel coating electrode, the enamel coating metallic matrix is low-carbon
Any one in steel, glassed steel or copper and copper alloy.
Further, in the preparation method step a of above-mentioned enamel coating electrode, the copper alloy is Cu-5Zn, Cu-5Sn
Or Cu-5Sn-5Zn any one.
Preferably, in the preparation method step a of above-mentioned enamel coating electrode, the conducting wire is copper core, aluminum core line or iron
Any one in core wire.Further, the conducting wire is copper core.
Preferably, in the preparation method step a of above-mentioned enamel coating electrode, the copper core cross-sectional area is 2~2.5mm2。
The copper core line length is 15~20cm.
Preferably, in the preparation method step a of above-mentioned enamel coating electrode, the welding uses Na2B4O7.4H2O and pine
Perfume auxiliary welding；Or it is directly adhesively fixed using conductive rubber.The conductive rubber includes copper glue, nickel glue, elargol, silver-colored carbon
Glue, carbon paste.
Specifically, in the preparation method step a of above-mentioned enamel coating electrode, the material of the container be rubber, plastics or
Any one in hard paper tube.Further, the material of the container is PVC material.
Specifically, in the preparation method step a of above-mentioned enamel coating electrode, the outer diameter of the PVC containers is 16~20mm.
Preferably, in the preparation method step b of above-mentioned enamel coating electrode, the curing agent is ethylenediamine, divinyl three
Any one in amine, dicyandiamide or polyisocyanates.Further, the curing agent is ethylenediamine.
Preferably, in the preparation method step b of above-mentioned enamel coating electrode, the plasticizer is two fourth of phthalic acid
Ester.
Further, in the preparation method step b of above-mentioned enamel coating electrode, the mass ratio of epoxy resin and ethylenediamine is
3.8~4:1.More preferably 4:1.
Further, in the preparation method step b of above-mentioned enamel coating electrode, epoxy resin and dibutyl phthalate
Mass ratio be 7.5~8:1.
Further, described that bubble removing is gone to use at 40~60 DEG C in the preparation method step b of above-mentioned enamel coating electrode
The mode of constant temperature is realized.
Specifically, in the preparation method step b of above-mentioned enamel coating electrode, it is described to remove in the mixture being added to the container
Bubble realization is moved back and forth along metallic matrix surrounding using hard filament.Using thin wire along metallic matrix surrounding edge back and forth
It is mobile, so that the bubble floating of surrounding is gone out the surface of epoxy resin liquid, then without bubble after solidification.
Second technical problem to be solved by this invention is to provide the enamel coating electrode being prepared by the above method.
Third technical problem to be solved by this invention is to provide the test method of enamel coating corrosion resistance.The test
Method includes the following steps：By above-mentioned enamel coating electrode, platinum electrode, calomel reference electrode and the electrochemical analysis being prepared
Instrument connects, and enamel coating electrode, platinum electrode, calomel reference electrode are put into etchant solution, is powered, measures polarization curve number
Value, makes Ecorr-logi(A/cm2) polarization curve, obtain corrosion potential EcorrWith corrosion electric current density icorr, while obtaining enamel
Coating corrosion rate V=3.27 (A.icorr)/(n.d)；
Wherein, icorr=i/S；I is by logi(A/cm2) logarithm of negating obtains；S is the surface area in enamel coating face；D is to ward off
Porcelain density, A are enamel mean atomic weight, and n is the electron transfer number of electro-chemical test.
Specifically, in the test method of above-mentioned enamel coating corrosion resistance, the etchant solution is conventional corrosion liquid.Such as
Acid solution, aqueous slkali, simulation 3%NaCl seawater.Different corrosive liquid corrosive powers is different, the corrosion potential of generation and
Corrosion current is just different, and the corrosion electric current density and corrosion rate value measured is also different.
Further, in the test method of above-mentioned enamel coating corrosion resistance, the acid solution be mass concentration 15~
20~30% sulfuric acid solution of 30% hydrochloric acid or mass concentration.
Specifically, in the test method of above-mentioned enamel coating corrosion resistance, the electrochemical analyser is CHI640 series
Or CHI660 series.
Preferably, in the test method of above-mentioned enamel coating corrosion resistance, control enamel coating electrode coat side towards
Platinum electrode and calomel reference electrode, distance are 1~2cm.
Preferably, in the test method of above-mentioned enamel coating corrosion resistance, the open circuit potential OCP-0.5 of test~-
0.85V.Testing time is 1200~1500s.
The present invention tests enamel coating corrosion resistance using electrochemical means, has easy to operate, time-consuming be as short as
The advantages that 20~30min, more accurate result.The present invention tests enamel coating corrosion resistance using electrochemical means, makes first
For a kind of enamel coating electrode.When preparing enamel coating electrode, by pre-treatments such as grindings, enamel coating and metal ensure that
The case where matrix flat side down, enamel coating are without de- porcelain, cracking, high yield rate；Simultaneously using epoxy resin and curing agent, plasticising
Agent seals other faces in addition to enamel coating, removes bubble etc., finally ensure that the accuracy of follow-up test.
Description of the drawings
Enamel coating electrode prepared by Fig. 1 present invention；
Working electrode needed for Fig. 2 enamel coating electrochemical corrosion tests of the present invention；
The working electrode location drawing that enamel coating electrochemical corrosion is tested in Fig. 3 present invention；
The connection figure of Fig. 4 electrochemical analyser test enamel coating electrochemical corrosion of the present invention；
Fig. 5 present invention tests the polarization curve of enamel coating electrochemical corrosion.
Specific implementation mode
In order to measure enamel coating corrosion resistance, for defect existing for existing method, the present invention then uses electrochemical credit
Analysis method measures the corrosion resistance of enamel coating.The present invention uses enamel coating to prepare enamel coating electrode for raw material first.
However due to the particularity of enamel coating, enamel coating is attached to metal base surface and is unable to individualism, first, if not right
It is handled, and metallic matrix necessarily affects measurement result；Meanwhile when preparing enamel coating, since the heat of enamel coating is swollen
The coefficient of thermal expansion of swollen rate and metallic matrix is close, and causing mechanical processing to make, difficult, yield rate is low, to which the present invention provides one
The method of kind special preparation enamel coating electrode.This method, as electrode bed, makes electrode cable using enamel coating by soldering
Element is connect with electrode bed, covers to form electrode bed protective film using epoxy resin, and opening is formed in protective film, so that
Enamel coating surface exposes in the opening, to complete required electro-chemical test.
The present invention can prepare enamel coating electrode using any enamel coating as sample to be tested using the method for the present invention, from
And measure the corrosion resistance of this kind of enamel coating.Further, the metallic matrix of the enamel coating be mild steel, glassed steel or
Any one in copper and copper alloy steel.Further, the copper alloy steel is to appoint in Cu-5Zn, Cu-5Sn or Cu-5Sn-5Zn
Meaning is a kind of.Specifically, present invention firstly provides the preparation method of enamel coating electrode, include the following steps：
(1) enamel coating cut, polished, being ground, being washed, absolute ethyl alcohol is washed or acetone washout goes water, drying standby
With；
(2) it in the metal base surface welding lead of step (1) pretreated enamel coating, will be integrally put into after welding
In PVC containers；
(3) bubble removing will be removed after epoxy resin, curing agent mixing, adds plasticizer mixing and obtain mixture, by mixture
It is added in the PVC containers of step (2) and is sealed other faces in addition to enamel coating face；
(4) bubble in the mixture in PVC models is added in removal, waits for epoxy resin cure, takes out, polishing, cleans, obtains
To enamel coating electrode.
In step (1), since enamel coating is that inorganic ceramic glaze is non-conductive, wire cutting, laser cutting, and one cannot be used
As emery wheel cuts when cutting force it is uneven, enamel coating is easy de- porcelain, cracking etc.；It is excellent in order to ensure the accuracy of subsequent detection
Choosing intercepts enamel coating sample using Metallographic Specimen Cutting Machine using high-speed rotating disc wheel, is produced when to prevent cutting
Raw heat avoids enamel coating sample heat and changes institutional framework, and when cutting opens chilled water unit.It is preferred that control cutting
Rotating speed be 2800~3000r/min.
In step (1), due to will produce flash after cutting, detection accuracy can be also influenced, then also needs to polish to it,
It is preferred that polishing rotating speed is 1200~1500r/min.It is water-cooled after every 3~5s, prevents the heat that friction generates from changing enamel group
Knit structure.Sample edge and wheel face are in 70~80 ° of angles when polishing, prevent enamel coating and grinding wheel resistance is excessive leads to enamel
Glaze layer falls off or cracks.It is preferred that being polished using abrasive machine.Polishing actually can not be also used, follow-up grinding can be used and come in fact
It is existing, it can only cause subsequently to grind quality that is more time-consuming, but not influencing entirely to prepare enamel coating electrode.
In step (1), use sand paper for 240~700CW Al2O3Sample surrounding is ground, sample is in 90 ° with sand paper face, is turned
Speed is 400~500r/min, is ground to enamel coating and metallic matrix flat side down, edge of the enamel coating without de- porcelain, cracking；
The metallic enamel sample back side is polished with sand paper, increases the degree of roughness on its surface.
In step (1), the length and shape of enamel coating metallic matrix are not particularly limited, because in order to ensure to survey
Accuracy is tried, other than enamel coating removing coating face, other five faces can be sealed, and test result only has with the area of coat side
It closes.So, more convenient, simple, cost-effective etc. in order to operate, control enamel coating metallic matrix is length of side 10mm~15mm
Square or rectangular.
In step (2), conducting wire is in order to which the instrument of enamel coating and follow-up test is connected energization.Conventional wires copper
Core wire, aluminum core line or iron core line.Since copper conductor resistance is small, conductive effect is good, the corrosion current sheet in electro-chemical test
Body is just very faint, is not easy to decay with copper conductor corrosion current, is copper core it is advantageous to conducting wire.To copper core diameter and length
Degree does not specially require.It is preferred that copper core cross-sectional area is S=2~2.5mm2.Length is 15~20cm.Copper core is removed when welding
The PVC insulating outer layers of 1~1.5cm of both ends expose metal copper core, and wherein one end is tapped with adz-eye hammer to flat, spare.Welding
When, by 50~75W electric iron be powered after, electric iron tip be placed on the metal covering at the enamel coating back side make metal covering together by
Heat after heating 10~15min, when electric iron tip takes on a red color, dips in a little rosin and contact solder stick is after solder stick fusing, will
The flat one end of copper core is welded on electric iron on the metal covering at the enamel coating back side.
Further, the metal at the above-mentioned enamel coating back side is if it is mild steel Q235 or glassed steel BTC245 matrixes, copper
Core is not easy to be welded on the metal covering at the enamel coating back side with electric iron, can be dipped in when electric iron heats a little
Na2B4O7.4H2O is placed on the metal covering at the enamel coating back side and heats together, waits for Na2B4O7.4H2After O crystal meltings electric iron after
Continue to dip in a little rosin and contact solder stick and be welded after solder stick fusing.
Further, copper core cannot still be welded on the metallic matrix mild steel Q235 or glassed steel at the enamel coating back side
On BTC245, the flat one end of copper core is bonded on the metallic matrix at the enamel coating back side using conductive rubber.Described leads
Electric colloid includes copper glue, nickel glue, elargol, silver-colored carbon paste, carbon paste.
In step (2), the effects of PVC containers is to contain subsequent epoxy resin, the material of container in addition to metal material,
His material, such as rubber, plastics, hard paper tube.It is preferred that PVC.The size of container is not particularly limited, it is only necessary to foot
Enough contain material.The square or rectangular for being length of side 10mm~15mm according to control enamel coating metallic matrix, preferably
The outer diameter for controlling the container is 16~20mm.The container length is 15~20mm length.By PVC cylinders in metallographical polishing machine
On with the Al of 240CW2O3Sand paper is ground to that both ends are smooth, and no crimping, burr wash with water, 40~60 DEG C of drying, spare.
In step (2), one section of cellotape is bonded on smooth, clean glass surface, length is according to preparation number of electrodes
Depending on, cellotape both ends are reversed, it is entirely sticked on glass surface, keeps remaining glue surface of cellotape upward, above-mentioned PVC is justified
Cylinder is upright, it is neat, be bonded in adhesive tape glue surface side by side, the above-mentioned enamel coating for being welded with copper core is put into PVC cylinders, is made
Enamel coating face is bonded on adhesive tape, and is in PVC cylinder center position, and one section of glue is bonded again at the upright copper core back side
Band, adhesive tape both ends are adhesively fixed with brandreth, and copper core is uprightly bonded on adhesive tape, prevent copper core enamel electrode from toppling over.
In step (3), in order to ensure the accuracy of subsequent detection, it need to will be sealed except other faces in enamel coating face.To warding off
Porcelain electrode is sealed, and used material demand is cured, and acid-alkali-corrosive-resisting again, so selection epoxy resin.
It is mixed with curing agent, plasticiser using epoxy resin and is used as sealing material.The curing agent is conventional solidified dose, such as second two
Any one in amine, diethylenetriamine, dicyandiamide or polyisocyanates.The plasticizer is Conventional plasticizers, such as plasticizer
For dibutyl phthalate.Since the bubble in sealing material can have an impact test, PVC containers are added in sealing material
Bubble removing is also needed afterwards, if curing agent addition is excessive, curing rate is too fast, fully cannot remove bubble and influence to survey
Test result, if curing agent addition is very few, then curing rate is excessively slow, or even cannot cure, and it is advantageous to epoxy resin and second two
The mass ratio of amine is 3.8~4:1.More preferably 4:1.The mass ratio of preferred epoxy and dibutyl phthalate is 7.5
~8：1.
In step (3), since plasticizer can accelerate epoxy resin cure, speed can be such that the bubble of electrode surrounding does not allow
Easily choose and begin to cure, to influence test result.So generally by epoxy resin and curing agent mixing in container, 40
~60 DEG C of constant temperature are to complete softening, and the bubble of the inside can just overflow, to remove bubble removing；Plasticizer simultaneously in another container
In 40~60 DEG C of constant temperature.Wait for that all floating disperses bubble in epoxy resin, by epoxy resin, curing agent and the plasticising in two containers
Agent is poured into after being mixed evenly in the PVC containers containing enamel coating, is moved back along metallic matrix surrounding edge by thin wire
It is dynamic, so that the bubble floating of surrounding is gone out the surface of epoxy resin liquid, prevents residual in electrode metal matrix surrounding after epoxy resin cure
There are bubbles.Plasticizer accelerates epoxy resin cure, and curing agent and plasticizer, which play, adjusts epoxy resin cure speed and intensity
Effect.
In step (4), after the solidification for 24 hours of epoxy resin electrode, the extra epoxy resin of container surrounding is removed, with 2000CW's
Al2O3Sand paper polishes 3~5min on metallographical polishing machine, then uses acetone or the viscose glue on washes of absolute alcohol enamel coating surface
Residue is positioned over spare in drier.
Secondly, the present invention also provides the test method of the above-mentioned enamel coating corrosion resistance being prepared, including it is following
Step：
(1) prepare etchant solution, such as acid solution, such as 15~30% hydrochloric acid of mass concentration or mass concentration 20~
30% sulfuric acid solution can prepare different solution systems as needed；
(2) electrochemical analyser, platinum electrode, calomel reference electrode, enamel coating electrode are connected by Fig. 4, is put into step (1)
In prepared etchant solution, wherein calomel electrode fills saturation KCl solution；Respectively leading for two electrodes is connected with electrode wires
Line, for enamel coating electrode end surface to platinum electrode and calomel reference electrode, distance is 1~2cm, places electrode by Fig. 3, and connect
Circuit；
(3) computer and electrochemical analyser power supply are opened, after work station preheats 10~15min, into electrochemical analysis
Instrument application software；
(4) the corrosion electricity of Control → Open circuit potential measuring electrodes is opened successively from drop-down menu
Place value, current potential surface sweeping rate are 0.001V/s；
(5) Setup → Techniques → Open circuit potential-Time are first turned on from drop-down menu,
Then OK is pressed to select；
(6) open Setup → Parameters successively from pull-down menu, select the potential measurement time for 1200~
Then 1500S presses OK and selects；
(7) enamel coating electrode open circuit potential OCP-0.5~-0.85V in solution system, stable 5min, current potential polarization,
50~70 μ A/cm of cathode current2, 1~2min is activated, the testing time is 1200~1500s, tests the corrosion polarization of enamel coating
Curve；
(8) polarization curve numerical value is tested out, E is made with Origin softwarescorr-logi(A/cm2) curve, from Ecorr-logi
(A/cm2) log at the point of intersection of tangents is read in curve graphi(A/cm2), logi(A/cm2) in A be current unit ampere, then ask
Antilogarithm is converted into i values divided by enamel coating area S (cm2), obtain corrosion electric current density icorr, according to V=3.27 (A.icorr)/
(n.d) the corrosion rate V of enamel coating is calculated；
Wherein, formula V=3.27 (A.icorr)/(n.d) in, d is enamel density, is 5.65g/cm3；A is the average original of enamel
Son amount is 1 × 106g/mol；N is the electron transfer number of electro-chemical test, average out to 2；V is the corrosion rate of enamel coating, single
Position is g/m2/h。
Corrosive liquid of the present invention is conventional corrosion liquid, such as acid solution, aqueous slkali, 3%NaCl seawater, different corruption
Erosion corrosion ability is different, and the corrosion potential and corrosion current of generation are just different, the corrosion electric current density measured and corrosion
Velocity amplitude is also different.Corrosion potential, corrosion current of the different enamel coatings in different corrosive liquids can be measured according to demand
And corrosion rate.
Embodiment 1
The preparation of enamel coating electrode：12mm × 12mm samples are prepared into using Copper substrate enamel coating, edge is beaten
Mill makes enamel coating flat side down, without de- porcelain, cracking.The enamel coating back side is ground, polishing, cleans, after copper core wire bonding,
It is put into pvc pipe tool.Epoxy resin and curing agent ethylene diamine 3.5 ﹕ in mass ratio, 1 mixings, 10min goes degasification at a temperature of being placed in 50 DEG C
Bubble is that 8 ﹕ 1 take dibutyl phthalate that asphalt mixtures modified by epoxy resin is added by epoxy resin and plasticizer phthalic acid dibutyl ester mass ratio
In the constant temperature mixed liquor of fat and ethylenediamine, it is uniformly mixed, then pours into PVC models, gently choose coating surrounding minute bubbles, floating is removed
It goes.Electrode solidification is taken out afterwards for 24 hours, and polished, anhydrous ethanol elution, drying are prepared into enamel coating electrode.
Acid corrosion-resistant is tested：Electrochemical analyser CHI660C is connected by Fig. 4, by platinum electrode, calomel reference electrode, is warded off
Porcelain coated electrode is put into polarization pond 20%HCl solution, is placed electrode by Fig. 3, is connected with electrode wires, working electrode enamel applies
To platinum electrode, distance is 1~2cm for level end face.It is -0.62V that open circuit potential OCP, which is arranged, by software, stablizes 5min, cathode electricity
Flow 50 μ A/cm2, 2min is activated, 1500s is tested, current potential surface sweeping rate is 0.001V/s, tests out the polarization curve of enamel coating
Numerical value makes E with Origin softwarescorr-logi(A/cm2) curve, see Fig. 5 curve a, the corruption of enamel coating is calculated by curve a
Lose current density icorrIt is 1.28 × 10-6μA/cm2, the corrosion rate V of enamel coating is 13.5g/m2/ h, the results are shown in Table 1.
Embodiment 2
The preparation of enamel coating electrode：12mm × 12mm samples, surrounding are prepared into using carbon steel Q235 matrix enamel coatings
Edge is polished, and makes enamel coating flat side down, without de- porcelain, cracking.The enamel coating back side is ground, polishing, cleans, copper core wire bonding
After connecing, it is put into pvc pipe tool.Epoxy resin and curing agent ethylene diamine 4 ﹕ in mass ratio, 1 mixings, 10min is gone at a temperature of being placed in 50 DEG C
Bubble removing takes dibutyl phthalate to be added with plasticizer phthalic acid dibutyl ester mass ratio by epoxy resin for 7.8 ﹕ 1
In the constant temperature mixed liquor of epoxy resin and ethylenediamine, it is uniformly mixed, then pours into pvc pipe, gently choose coating surrounding minute bubbles, on
It is floating to remove.Electrode solidification is taken out afterwards for 24 hours, and polished, anhydrous ethanol elution, drying are prepared into enamel coating electrode.
Acid corrosion-resistant is tested：Electrochemical analyser CHI660C is connected by Fig. 4, by platinum electrode, calomel reference electrode, is warded off
Porcelain coated electrode is put into polarization pond 30%HCl solution, is placed electrode by Fig. 3, is connected with electrode wires, working electrode enamel applies
To platinum electrode, distance is 1~2cm for level end face.It is -0.65V that open circuit potential OCP, which is arranged, by software, stablizes 5min, cathode electricity
Flow 50 μ A/cm2, 2min is activated, 1500s is tested, current potential surface sweeping rate is 0.001V/s, tests out the polarization curve of enamel coating
Numerical value makes E with Origin softwarescorr-logi(A/cm2) curve, Fig. 5 curve b calculate the corrosion of enamel coating by curve b
Current density icorrIt is 1.46 × 10-6μA/cm2, the corrosion rate of enamel coating is 15.4g/m2/ h, the results are shown in Table 1.
Embodiment 3
The preparation of enamel coating electrode：12mm × 12mm samples are prepared into using glassed steel BTC245 matrix enamel coatings,
Edge is polished, and makes enamel coating flat side down, without de- porcelain, cracking.The enamel coating back side is ground, polishing, cleans, copper core
After wire bonding, it is put into pvc pipe tool.Epoxy resin and curing agent ethylene diamine 4 ﹕ in mass ratio, 1 mixings, are placed at a temperature of 50 DEG C
10min removes bubble removing, is that 8 ﹕ 1 take dibutyl phthalate by epoxy resin and plasticizer phthalic acid dibutyl ester mass ratio
It is added in the constant temperature mixed liquor of epoxy resin and ethylenediamine, is uniformly mixed, then pours into pvc pipe, it is stingy gently to choose coating surrounding
Bubble floats and removes.Electrode solidification is taken out afterwards for 24 hours, and polished, anhydrous ethanol elution, drying are prepared into enamel coating electrode.
Acid corrosion-resistant is tested：Electrochemical analyser CHI660C is connected by Fig. 4, by platinum electrode, calomel reference electrode, is warded off
Porcelain coated electrode is put into polarization pond 20%H2SO4In solution, electrode is placed by Fig. 3, is connected with electrode wires, working electrode enamel
To platinum electrode, distance is 1~2cm for face end face.It is -0.68V that open circuit potential OCP, which is arranged, by software, stablizes 5min, cathode current
50μA/cm2, 2min is activated, 1500s is tested, current potential surface sweeping rate is 0.001V/s, tests out the polarization curve number of enamel coating
Value, E is made with Origin softwarescorr-logi(A/cm2) curve, see Fig. 5 curve c, the corrosion of enamel coating is calculated by curve c
Current density icorrIt is 2.17 × 10-5μA/cm2, the corrosion rate of enamel coating is 229g/m2/ h, the results are shown in Table 1.
Embodiment 4
The preparation of enamel coating electrode：12mm × 12mm samples are prepared into using glassed steel BTC245 matrix enamel coatings,
Edge is polished, and makes enamel coating flat side down, without de- porcelain, cracking.The enamel coating back side is ground, polishing, cleans, copper core
After wire bonding, it is put into pvc pipe tool.Epoxy resin and curing agent ethylene diamine 4 ﹕ in mass ratio, 1 mixings, are placed at a temperature of 50 DEG C
10min removes bubble removing, is that 8 ﹕ 1 take dibutyl phthalate by epoxy resin and plasticizer phthalic acid dibutyl ester mass ratio
It is added in the constant temperature mixed liquor of epoxy resin and ethylenediamine, is uniformly mixed, then pours into pvc pipe, it is stingy gently to choose coating surrounding
Bubble floats and removes.Electrode solidification is taken out afterwards for 24 hours, and polished, anhydrous ethanol elution, drying are prepared into enamel coating electrode.
Acid corrosion-resistant is tested：Electrochemical analyser CHI660C is connected by Fig. 4, by platinum electrode, calomel reference electrode, is warded off
Porcelain coated electrode is put into polarization pond 30%H2SO4In solution, electrode is placed by Fig. 3, is connected with electrode wires, working electrode enamel
To platinum electrode, distance is 1~2cm for face end face.It is -0.7V that open circuit potential OCP, which is arranged, by software, stablizes 5min, cathode current
50μA/cm2, 2min is activated, 1500s is tested, current potential surface sweeping rate is 0.001V/s, tests out the polarization curve number of enamel coating
Value, E is made with Origin softwarescorr-logi(A/cm2) curve, see Fig. 5 curve d, the corrosion of enamel coating is calculated by curve d
Current density icorrIt is 2.75 × 10-5μA/cm2, the corrosion rate of enamel coating is 291g/m2/ h, the results are shown in Table 1.
Table 1
| Embodiment | Ecorr(v) | logi(A/cm2) | S(cm2) | icorr/(μA/cm2) | V(g/m2/h) |
| 1 | -0.622 | -11.72 | 1.483 | 1.28×10-6 | 13.5 |
| 2 | -0.646 | -11.68 | 1.432 | 1.46×10-6 | 15.4 |
| 3 | -0.686 | -10.58 | 1.213 | 2.17×10-5 | 229 |
| 4 | -0.714 | -10.49 | 1.176 | 2.75×10-5 | 291 |
The present invention quantitatively tests the corrosion current and corrosion rate of enamel coating using electrochemical method, changes biography
System enamel coating corrosion resistance test method, with easy to operate, the time is short, high accuracy for examination.
Claims (10)
1. the preparation method of enamel coating electrode, it is characterised in that：Include the following steps：
A, conducting wire is welded to the metal base surface of enamel coating, then put it into container；
B, epoxy resin and curing agent mixing are removed into bubble removing, adds plasticizer mixing and obtain mixture, adds mixture into step
Other faces in addition to enamel coating face are sealed in the container of rapid a；
C, the bubble in the mixture that removal is added to the container, waits for epoxy resin cure, obtains enamel coating electrode.
2. the preparation method of enamel coating electrode according to claim 1, it is characterised in that：In step a, the enamel applies
Layer need to be cut, be ground, being cleaned, dry after welded again.
3. the preparation method of enamel coating electrode according to claim 2, it is characterised in that：At least meet with the next item down：
The rotating speed of the cutting is 2800~3000r/min；
The equipment used is cut as Metallographic Specimen Cutting Machine；
The sand paper used that grinds is 240~700CW Al2O3, rotating speed is 400~500r/min；
Sample and sand paper face are in 90 ° when grinding；
The equipment used is ground as metallographical polishing machine；
It polishes before grinding；
The polishing rotating speed is 1200~1500r/min, and sample edge is in 70~80 ° of angles with wheel face；
The equipment used polish as abrasive machine；
The cleaning is first to wash, then washed with acetone or absolute ethyl alcohol.
4. according to the preparation method of claims 1 to 3 any one of them enamel coating electrode, it is characterised in that：In step a,
The enamel coating metallic matrix is any one in mild steel, glassed steel or copper and copper alloy；Preferably, the copper alloy is
Cu-5Zn, Cu-5Sn or Cu-5Sn-5Zn any one.
5. according to the preparation method of Claims 1 to 4 any one of them enamel coating electrode, it is characterised in that：In step b,
The curing agent is any one in ethylenediamine, diethylenetriamine, dicyandiamide or polyisocyanates；Preferred consolidation agent is second two
Amine；The plasticizer is dibutyl phthalate.
6. the preparation method of enamel coating electrode according to claim 5, it is characterised in that：In step b, epoxy resin with
The mass ratio of ethylenediamine is 3.8~4:1；Preferably 4:1；The mass ratio of epoxy resin and dibutyl phthalate be 7.5~
8:1。
7. according to the preparation method of claim 1~6 any one of them enamel coating electrode, it is characterised in that：In step b,
It is described to go bubble removing using realizing by the way of 40~60 DEG C of constant temperature；It is described to remove the mixture being added to the container in step c
In bubble moved back and forth along metallic matrix surrounding to realize using hard filament.
8. the enamel coating electrode being prepared by any one of claim 1~7 preparation method.
9. the test method of enamel coating corrosion resistance, it is characterised in that：Include the following steps：It is warded off according to any one of claims 8
Porcelain coated electrode, platinum electrode, calomel reference electrode and electrochemical analyser connect, and enamel coating electrode, platinum electrode, calomel are joined
It is put into etchant solution than electrode, is powered, measures polarization curve numerical value, make Ecorr-logi(A/cm2) polarization curve, obtain corruption
Lose current potential EcorrWith corrosion electric current density icorr, obtain corrosion rate V=3.27 (A.icorr)/(n.d)；
Wherein, icorr=i/S, i is by logi(A/cm2) logarithm of negating obtains；S is the surface area in enamel coating face；D is that enamel is close
Degree, A are enamel mean atomic weight, and n is the electron transfer number of electro-chemical test.
10. the test method of enamel coating corrosion resistance according to claim 9, it is characterised in that：The open circuit electricity of test
Position OCP-0.5~-0.85V；Testing time is 1200~1500s.
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