CN102735601A - Method for measuring coating corrosion-resistant properties - Google Patents
Method for measuring coating corrosion-resistant properties Download PDFInfo
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- CN102735601A CN102735601A CN2011100877490A CN201110087749A CN102735601A CN 102735601 A CN102735601 A CN 102735601A CN 2011100877490 A CN2011100877490 A CN 2011100877490A CN 201110087749 A CN201110087749 A CN 201110087749A CN 102735601 A CN102735601 A CN 102735601A
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- coating
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- decay resistance
- thickness
- capacitance
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Abstract
The invention discloses a method for measuring coating corrosion-resistant properties, wherein the coating corrosion-resistant properties are represented by measuring coating capacitances. The method concretely comprises immersing the surface of a part of the coating into the bottom of a corrosive solution to enable a conductive substrate under the coating and the corrosive solution to form a plate capacitor. The capacitance values of the plate capacitor are related to the thicknesses of the coating, so coating thickness changes can be determined by measuring capacitance value changes of the plate capacitor, and thus the coating corrosion-resistant properties can be quantitatively reflected according to the coating thickness changes which take place over-time. Compared with conventional measuring methods, the method is characterized by enlarging the scope of measurable coatings, being particularly suitable for measuring coating materials with high resistances and being insensitive to contamination of the coating materials. Moreover, the measuring method is sensitive in response, capable of rapidly reflecting coating corrosion states for the materials.
Description
Technical field
The present invention relates to the coating field of measuring technique, particularly a kind of method of measuring the coating decay resistance.
Background technology
At present; The low temperature plasma microfabrication has become the gordian technique of material micro-nano processing; Because it is the basis of technologies of preparing such as microelectronics, photoelectron, micromechanics, micro-optic; Particularly in the VLSI (very large scale integrated circuits) manufacturing process, there is nearly 1/3rd operation to accomplish, like plasma foil deposition, plasma etching and removing of photoresist by plasma etc. by means of plasma process; Wherein plasma etching is one of the most key technological process, is with high fidelity to transfer to the irreplaceable technology on the silicon chip from Lithographic template by Micropicture in the VLSI (very large scale integrated circuits) production.
In plasma etch process, at first be on silicon wafer, to smear the photoactive substance that one deck is made up of hydrocarbon, and have the metal form of certain figure rule at photoactive substance loam cake last layer; Carry out uv-exposure then, make the wafer surface of exposed portion expose out; Then be placed into silicon wafer to be processed again and have in the chemically active low temperature plasma, carry out plasma etching.This have that chemically active plasma normally produces by chlorine or carbon fluorine gas discharge, and it not only contains electronics and ion, also contain a large amount of living radicals (like Cl*, Cl
2*, F*, CF* etc.).When these reactive groups deposited on the exposed silicon wafer, they combined with silicon atom and form volatile silicon chloride or silicon fluoride molecule, thereby wafer is carried out anisotropic etching.
Distribute and angle distribution in order to control the energy of ions of bombarding on the wafer, usually wafer is placed on above the electrode that applies radio frequency or pulsed bias, above wafer, will form non-electroneutral plasma slab, i.e. a sheath layer like this.Ion in the plasma is bombarded on the exposed wafer surface under sheath layer effect of electric field, and collides with the silicon atom of superficial layer, it is sputtered out, thereby realize the anisotropic etching to wafer.Because in etching process, generated a large amount of have corrosive living radical (like Cl*, Cl
2*, F*, CF* etc.), the inside surface of meeting article on plasma etching technics cavity produces corrosive attack, has brought pollution to chamber, has influenced etching effect, and the protective seam in the etching technics chamber was lost efficacy because of being destroyed.
In the plasma etching equipment of the nineties in last century in early days, take place under the situation in source at smaller power and single plasma, as long as the aluminum substrate layer adds Al
2O
3Coating just can satisfy the requirement of plasma to the etch damage in etching technics chamber.But the continuous increase along with the dimensions of wafer especially increases to after the 300mm, and the plasma power of relevant device also increases thereupon, and plasma is also increasing to the damage of etching technics chamber wall, and yttria (Y
2O
3) basic coating has the performance that higher anti-plasma corrodes because of it, and the protective seam that is applied to the etching technics chamber gradually.Be used for the coating in etching technics chamber to above these; Need carry out the measurement of decay resistance to it; And common measuring method is to characterize its corrosion resistance with the resistance variations of coating in etchant solution; But because these coating materials are insulator, so the application of existing electric-resistivity method is restricted, and its response speed to etch state is very slow.
Summary of the invention
The technical matters that (one) will solve
The present invention is directed to the existing problem of resistance measurement coating decay resistance, proposed a kind of method of measuring the coating decay resistance.
(2) technical scheme
For achieving the above object; The invention provides a kind of method of measuring the coating decay resistance; This method is to utilize the method for measuring coating capacitor to come the characterizing coating decay resistance; Specifically comprise: earlier the surface of a part of coating is dipped in the bottom of corrosive solution, makes conducting base and corrosive solution under the coating constitute a plate condenser, the capacitance of this plate condenser is relevant with the thickness of coating; Confirm the variation of coating thickness to reflect corrosion resistance of coating over time quantitatively through the variation of measuring this plate condenser capacitance according to coating thickness.
(3) beneficial effect
Compare with existing measuring technique, characteristics of the present invention are that the scope of measuring coating increases, and are particularly suitable for measuring high-resistance coating material, and insensitive to the pollution of coating material.The reaction velocity of this measuring method is sensitive in addition, can reflect the etch state of material coating rapidly.
Description of drawings
Fig. 1 is for measuring the device synoptic diagram of coating decay resistance according to the embodiment of the invention.
Embodiment
For making the object of the invention, technical scheme and advantage clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, to further explain of the present invention.
The porosity of hot spray coating is usually between 3-15%, thereby this imperfection can cause some chemicals can penetrate and arrive coating was lost efficacy or coming off of coating and matrix.
For example, can find the accessory substance AlCl of etching for the parts that are applied in the aluminium etching cavity
3Can generate acid with airborne water molecule reaction, reaction equation is:
2AlCl
3+3H
2O＝2Al(OH)
3+6HCl
The rare earth oxide that the plasma thermal sprayed method obtains (Y for example
2O
3) coating has the volume porosity about 5%, what HCl will penetrate that these pores arrive coatings and matrix attacks the rare earth oxide coating at the interface and at this at the interface, thereby causes coating and high base strength reduction.
And for using anodised aluminium substrate, because anodic oxide coating itself is very sparse, HCl can arrive aluminium base lamella through the crack in the anodic oxide coating, thereby causes a chemical reaction that produces hydrogen to take place, and reaction equation is:
2Al+6HCl＝2AlCl
3+3H
2
And reaction product AlCl
3Can produce reaction with airborne hydrone again and generate HCl, the next circulation of beginning.When between aluminum substrate and the coating have abundant hydrogen at the interface the time, will form gas cavity, after having formed enough big pressure, can cause coating to receive very big infringement, finally can cause coming off of coating.
After coating is carried out wet cleaning, if, will have hydrone residual without baking fully.In etching subsequently, Cl
2Generate HCl with water molecule reaction, this will cause peeling off of coating.
Based on above-mentioned realization principle; The method of measurement coating decay resistance provided by the invention; Be to utilize the method for measuring coating capacitor to come the characterizing coating decay resistance; Specifically comprise: earlier the surface of a part of coating is dipped in the bottom of corrosive solution, makes conducting base and corrosive solution under the coating constitute a plate condenser, the capacitance of this plate condenser is relevant with the thickness of coating; Confirm the variation of coating thickness through the variation of measuring this plate condenser capacitance, thereby reflect corrosion resistance of coating over time quantitatively according to coating thickness.
Wherein, the material of said coating employing is an insulating ceramic materials.Said corrosive solution is acidity or alkaline solution.Said conducting base is metal, alloy or other solid-state conductive material.The capacitance of said plate condenser is relevant with the thickness of coating, is by formula C=ε
0ε
rS/d characterizes, and wherein C is the capacitance of plate condenser, ε
0Be permittivity of vacuum, ε
rBe the specific inductive capacity of coating material, S is the area that is dipped in the coating surface of corrosive solution, and d is the thickness of coating.
Said according to coating thickness reflect corrosion resistance of coating over time quantitatively, for example: in order to measure pottery (Y for example
2O
3) corrosion resistance of coating, being placed in the HCl solution of 1-20at%, Fig. 1 is for measuring the device synoptic diagram of coating decay resistance according to the embodiment of the invention.Y
2O
3Coating 12 is a coating to be measured, and chamber wall 13 is installed in Y
2O
3On the surface of coating 12, HCl solution 14 is put into chamber wall 13.With a lead 15 aluminium substrate 11 is linked to each other with C meter 17, C meter 17 is linked to each other with platinum electrode 18 in the HCl solution 14 with another root lead 16.The electrode that aluminium substrate and HCl solution constitute can be regarded a plate condenser simply as, and C meter 17 is used for measuring the electric capacity of coating, the relation below it satisfies:
C＝ε
0ε
rS/d
Wherein C is the capacitance of plate condenser, ε
0Be permittivity of vacuum, ε
rBe the specific inductive capacity of coating material, S is the area that is dipped in the coating surface of corrosive solution, is the area that is dipped in the coating in the HCl solution 14, and d is the thickness of coating.
By the visible prolongation along with etching time of the formula of electric capacity, coating is with attenuation, and correspondingly electric capacity will increase.The corrosion rate of coating can be detected quantitatively over time through electric capacity, thereby the decay resistance of coating material can be obtained.
Above-described specific embodiment; The object of the invention, technical scheme and beneficial effect have been carried out further explain, and institute it should be understood that the above is merely specific embodiment of the present invention; Be not limited to the present invention; All within spirit of the present invention and principle, any modification of being made, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. a method of measuring the coating decay resistance is characterized in that, this method is to utilize the method for measuring coating capacitor to come the characterizing coating decay resistance, specifically comprises:
Earlier the surface of a part of coating is dipped in the bottom of corrosive solution; Make conducting base and corrosive solution under the coating constitute a plate condenser; The capacitance of this plate condenser is relevant with the thickness of coating; Confirm the variation of coating thickness to reflect corrosion resistance of coating over time quantitatively through the variation of measuring this plate condenser capacitance according to coating thickness.
2. the method for measurement coating decay resistance according to claim 1 is characterized in that, the material that said coating adopts is an insulating ceramic materials.
3. the method for measurement coating decay resistance according to claim 1 is characterized in that, said corrosive solution is acidity or alkaline solution.
4. the method for measurement coating decay resistance according to claim 1 is characterized in that, said conducting base is a metal or alloy.
5. the method for measurement coating decay resistance according to claim 1 is characterized in that, the capacitance of said plate condenser is relevant with the thickness of coating, is by formula C=ε
0ε r
S/ d characterizes, and wherein C is the capacitance of plate condenser, ε
0Be permittivity of vacuum, ε
rBe the specific inductive capacity of coating material, S is the area that is dipped in the coating surface of corrosive solution, and d is the thickness of coating.
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|---|---|---|---|
| CN2011100877490A CN102735601A (en) | 2011-04-08 | 2011-04-08 | Method for measuring coating corrosion-resistant properties |
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|---|---|---|---|
| CN2011100877490A CN102735601A (en) | 2011-04-08 | 2011-04-08 | Method for measuring coating corrosion-resistant properties |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103728239A (en) * | 2014-01-02 | 2014-04-16 | 国家电网公司 | Non-contact type coating failure detection system and method |
| CN104062194A (en) * | 2013-03-18 | 2014-09-24 | 深圳市海洋王照明工程有限公司 | Testing method of lamp coating wear resistance |
| TWI467150B (en) * | 2013-06-05 | 2015-01-01 | Univ Dayeh | Method of detecting anti-fluoride corrosion resistance of anodically oxidized aluminum film |
| CN107178538A (en) * | 2017-06-07 | 2017-09-19 | 中国科学技术大学 | A kind of capacitance type detector of guidance tape wear extent |
| CN111238358A (en) * | 2020-02-25 | 2020-06-05 | 山东大学 | Resistance value test-based cutter coating thickness measuring electrode, device and method |
| CN112947136A (en) * | 2021-01-16 | 2021-06-11 | 河南检亿科技有限公司 | Intelligent monitoring device for aging degree of steel lining storage tank, monitoring process and method |
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2011
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104062194A (en) * | 2013-03-18 | 2014-09-24 | 深圳市海洋王照明工程有限公司 | Testing method of lamp coating wear resistance |
| TWI467150B (en) * | 2013-06-05 | 2015-01-01 | Univ Dayeh | Method of detecting anti-fluoride corrosion resistance of anodically oxidized aluminum film |
| CN103728239A (en) * | 2014-01-02 | 2014-04-16 | 国家电网公司 | Non-contact type coating failure detection system and method |
| CN103728239B (en) * | 2014-01-02 | 2015-11-04 | 国家电网公司 | A kind of contactless coating failure detection system and detection method |
| CN107178538A (en) * | 2017-06-07 | 2017-09-19 | 中国科学技术大学 | A kind of capacitance type detector of guidance tape wear extent |
| CN111238358A (en) * | 2020-02-25 | 2020-06-05 | 山东大学 | Resistance value test-based cutter coating thickness measuring electrode, device and method |
| CN112947136A (en) * | 2021-01-16 | 2021-06-11 | 河南检亿科技有限公司 | Intelligent monitoring device for aging degree of steel lining storage tank, monitoring process and method |
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Application publication date: 20121017 |