CN104792291A - Method for precisely measuring thickness of thin macromolecular coating layer - Google Patents
Method for precisely measuring thickness of thin macromolecular coating layer Download PDFInfo
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- CN104792291A CN104792291A CN201510204701.1A CN201510204701A CN104792291A CN 104792291 A CN104792291 A CN 104792291A CN 201510204701 A CN201510204701 A CN 201510204701A CN 104792291 A CN104792291 A CN 104792291A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B21/00—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant
- G01B21/02—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness
- G01B21/08—Measuring arrangements or details thereof, where the measuring technique is not covered by the other groups of this subclass, unspecified or not relevant for measuring length, width, or thickness for measuring thickness
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Abstract
The invention discloses a method for precisely measuring thickness of a thin macromolecular coating layer. The method includes: taking a silicon wafer with the surface polished as a carrier material, and cutting the silicon wafer in a proper size to serve as a sample carrier; preparing a macromolecular coating layer on the sample carrier by adoption of a preparation process identical to that of the to-be-measured macromolecular coating layer; partially removing the coating layer on the carrier to expose the surface of the carrier; using a high-precision contourgraph to scan the surface of the to-be-measured sample and the surface of the sample carrier so as to obtain a height scan curve according to height changes, wherein a height represented by the height scan curve is equal to the thickness of the thin macromolecular coating layer. By adoption of the method, thicknesses of thin macromolecular coating layers with the thicknesses ranging from 100 nanometers to 10 micrometers can be measured accurately. In addition, the method for precisely measuring the thickness of the thin macromolecular coating layer is simple.
Description
Technical field
Embodiments of the present invention relate to material properties test technical field, and more specifically, embodiments of the present invention relate to the method for a kind of accurate test thickness at the slim polymeric coating layer thickness of 100nm-10 μm.
Background technology
Coating thickness is one of important indicator weighing polymeric coating layer preparation quality, be related to the THICKNESS CONTROL, raw materials consumption, serviceable life, substrate combinating strength etc. of preparing polymeric coating layer on the one hand, on the other hand in the correlative study such as crystallization degree, thermophysical property, mechanical behavior carrying out macromolecule membrane, also need the accurate data obtaining its thickness.Method for testing precision for thin coating thickness comprises: ultrasonic, eddy current, magnetic induction, laser etc., but these methods are mainly suitable for metallic coating, also there is limitation when being applied to polymeric coating layer.At present the on-line monitoring methods such as quartz transducer are generally adopted, based on the direct method of testing of clock gauge equal thickness for polymeric coating layer, wherein the on-line monitoring result such as quartz transducer often also adopts clock gauge method of testing to calibrate, and these methods are suitable only for thicker polymeric coating layer test.If slim polymeric coating layer thickness is less than 10 μm when being even less than 100nm, because clock gauge selftest error is greater than 1um, the error of the coating thickness of the method test is too large, and is also inaccurate based on the method for the calibration result of the film thickness monitors such as quartz.
The present invention proposes slim polymeric coating layer to be prepared in the regional area that a piece has the sample stage of high surface finish, utilize the method for high-precision surface contourgraph testing film and sample stage surface height difference to test, preparation quality sign, performance study etc. that the method can be slim polymeric coating layer on the one hand provide thickness data accurately, also may be used for the calibration of the film thickness monitor in thin coating preparation process in addition.
Summary of the invention
What the present invention is directed to the slim polymeric coating layer thickness of thickness between 100nm-10 μm is difficult to accurate test problem, propose the method for testing based on high-accurate outline instrument, determined the sample stage material selection in the method, preparation method of sample, coating surface and sample stage surface height difference method of testing, coating thickness calculating method etc. by test.
For solving above-mentioned technical matters, one embodiment of the present invention by the following technical solutions:
A method for the slim polymeric coating layer thickness of accurate test, it comprises the following steps:
The preparation of A, sample stage
Choose the silicon chip of surface through polishing as sample stage material, then described silicon chip is cut to the size being convenient to prepare sample coatings and carry out instrument test, obtains sample stage;
The preparation of B, testing sample
According to the preparation technology identical with polymeric coating layer to be measured, described sample stage prepares polymeric coating layer, after preparation, described polymeric coating layer is removed area, and on sample stage, remaining polymeric coating layer is testing sample;
The measurement of C, coating surface and sample stage surface height difference
Measuring accuracy is adopted to be less than the high-accurate outline instrument scanning testing sample surface of 0.01nm and the height change on sample stage surface, record height scan curve;
The calculating of D, testing sample thickness
Make two height parallel lines along two horizontal lines on described height scan curve, calculate the difference in height △ H between two height parallel lines, △ H is the thickness of slim polymeric coating layer sample to be measured.
In the method for the slim polymeric coating layer thickness of accurate test of the present invention, described surface is less than 0.5nm through the surfaceness of the silicon chip of polishing.
In the method for the slim polymeric coating layer thickness of accurate test of the present invention, the sample stage surface solvent cleaning exposed after described sample stage being removed the polymeric coating layer of area.
In the method for the slim polymeric coating layer thickness of accurate test of the present invention, described solvent is the solvent not dissolving slim polymeric coating layer.
According to one embodiment of the present invention, described solvent is alcohol or distilled water.
In the method for the slim polymeric coating layer thickness of accurate test of the present invention, before described sample stage prepares polymeric coating layer, first surface preparation or covering are carried out in the area region of described sample stage, reduce the bond strength of this region polymeric coating layer and sample stage.
Described surface preparation refers to the area adopting silicone oil or adhesive sticker coated sample microscope carrier.
In the method for the slim polymeric coating layer thickness of accurate test of the present invention, described area is at least 1/3 of the area of polymeric coating layer or sample stage, the half of the area of such as polymeric coating layer or sample stage.
Compared with prior art, one of beneficial effect of the present invention is: table 1 is the test value of the different-thickness coating adopting the method test, and carry out the contrast of the test result of the quartzy thickness on-line computing model calibrated with employing clock gauge, from test result, compare with high-precision surface contourgraph test result, the test data of quartzy film thickness monitor is significantly bigger than normal, needs according to high-accurate outline instrument test result, again check and debug, visible test result of the present invention is relatively more accurate.
Table 1 high-accurate outline instrument compares with quartzy film thickness monitor thickness measuring result
Accompanying drawing explanation
Fig. 1 is polymeric coating layer thickness measuring sample schematic diagram of the present invention.
Fig. 2 is coating surface of the present invention and the typical curve without the height change on coating area sample stage surface.。
Fig. 3 is coating thickness calculating method schematic diagram of the present invention.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
The thickness of what the present embodiment will be tested is polyurethane thin layer.First make the roughness of silicon chip surface be less than 0.5nm through polishing on the surface of silicon chip, be then cut into the size of 20mm × 20mm, obtain sample stage; According to the preparation technology that this polymer electrolyte thin layer is identical, sample stage prepares identical polymer electrolyte thin layer; Remove the polymer electrolyte thin layer of half area on silicon chip and expose the surface of this region samples microscope carrier, if when polymer electrolyte thin layer and silicon chip bond strength are not very high, can directly remove; If polymer electrolyte thin layer and silicon chip bond strength high, when being not easy to remove, can first silicon chip half surface area be first coated with one deck silicone oil or hide before plating polymer electrolyte thin layer, reduce bond strength between coating and silicon chip, then use the surface in this region of alcohol washes sample stage.After preparation, sample to be tested as shown in Figure 1, and polymer electrolyte thin layer 1 only accounts for the area of sample at platform 2 after making.
The above-mentioned sample to be tested prepared is placed on the test board of high-accurate outline instrument, require that the measuring accuracy of high-accurate outline instrument is less than 0.01nm, and energy acquisition and recording height scan curve, polymer electrolyte thin layer surface and the height change without the sample stage surface in polymer electrolyte thin layer region on test sample to be tested, record height scan curve.Fig. 2 be on a test sample without polymer electrolyte thin layer coating area with without the typical curve of the height change of coating area.
Two height parallel lines are made according to the parallel lines region of two on height scan curve, one the wherein height representing sample to be tested coating area, another represents the height without coating area, test the difference in height △ H between these two parallel lines, be polymer electrolyte thin layer thick coating angle value, see Fig. 3.
The difference in height △ H that the present embodiment records is 10 μm, and the thickness of polyurethane high molecule thin layer that namely the present embodiment will be tested is 10 μm.
Embodiment 2
The thickness of what the present embodiment will be tested is Parylene C thin layer.First make the roughness of silicon chip surface be less than 0.5nm through polishing on the surface of silicon chip, be then cut into the size of 15mm × 20mm, obtain sample stage; First silicon chip half surface area is hidden before plating polymer electrolyte thin layer, then according to the preparation technology that this polymer electrolyte thin layer is identical, sample stage is prepared identical polymer electrolyte thin layer; Remove the polymer electrolyte thin layer of half area on silicon chip and expose the surface of this region samples microscope carrier, then with the surface in distilled water cleaning this region of sample stage.
The above-mentioned sample to be tested prepared is placed on the test board of high-accurate outline instrument, the measuring accuracy of high-accurate outline instrument is less than 0.01nm, and energy acquisition and recording height scan curve, polymer electrolyte thin layer surface and the height change without the sample stage surface in polymer electrolyte thin layer region on test sample to be tested, record height scan curve.
Two height parallel lines are made according to the parallel lines region of two on height scan curve, one the wherein height representing sample to be tested coating area, another represents the height without coating area, tests the difference in height △ H between these two parallel lines, is polymer electrolyte thin layer thick coating angle value.
The difference in height △ H that the present embodiment records is 100nm, and the thickness of Parylene C polymer electrolyte thin layer that namely the present embodiment will be tested is 100nm.
Embodiment 3
The thickness of what the present embodiment will be tested is polyurethane thin layer.First make the roughness of silicon chip surface be less than 0.5nm through polishing on the surface of silicon chip, be then cut into the size of 22mm × 20mm, obtain sample stage; First silicon chip half surface area is hidden before plating polymer electrolyte thin layer, then according to the preparation technology that this polymer electrolyte thin layer is identical, sample stage is prepared identical polymer electrolyte thin layer; Remove the polymer electrolyte thin layer of half area on silicon chip and expose the surface of this region samples microscope carrier, then using the surface in this region of alcohol washes sample stage.
The above-mentioned sample to be tested prepared is placed on the test board of high-accurate outline instrument, the measuring accuracy of high-accurate outline instrument is less than 0.01nm, and energy acquisition and recording height scan curve, polymer electrolyte thin layer surface and the height change without the sample stage surface in polymer electrolyte thin layer region on test sample to be tested, record height scan curve.
Two height parallel lines are made according to the parallel lines region of two on height scan curve, one the wherein height representing sample to be tested coating area, another represents the height without coating area, tests the difference in height △ H between these two parallel lines, is polymer electrolyte thin layer thick coating angle value.
The difference in height △ H that the present embodiment records is 3 μm, and the thickness of polyurethane high molecule thin layer that namely the present embodiment will be tested is 3 μm.
Although with reference to multiple explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of, accompanying drawing open in the application and claim, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (8)
1. accurately test a method for slim polymeric coating layer thickness, it is characterized in that it comprises the following steps:
The preparation of A, sample stage
Choose the silicon chip of surface through polishing as sample stage material, then described silicon chip is cut to the size being convenient to prepare sample coatings and carry out instrument test, obtains sample stage;
The preparation of B, testing sample
According to the preparation technology identical with polymeric coating layer to be measured, described sample stage prepares polymeric coating layer, after preparation, described polymeric coating layer is removed area, and on sample stage, remaining polymeric coating layer is testing sample;
The measurement of C, coating surface and sample stage surface height difference
Measuring accuracy is adopted to be less than the high-accurate outline instrument scanning testing sample surface of 0.01nm and the height change on sample stage surface, record height scan curve;
The calculating of D, testing sample thickness
Make two height parallel lines along two horizontal lines on described height scan curve, calculate the difference in height △ H between two height parallel lines, △ H is the thickness of slim polymeric coating layer sample to be measured.
2. the method for the slim polymeric coating layer thickness of accurate test according to claim 1, is characterized in that described surface is less than 0.5nm through the surfaceness of the silicon chip of polishing.
3. the method for the slim polymeric coating layer thickness of accurate test according to claim 1, the sample stage surface solvent cleaning exposed after it is characterized in that described sample stage removes the polymeric coating layer of area.
4. the method for the slim polymeric coating layer thickness of accurate test according to claim 3, is characterized in that described solvent is the solvent not dissolving slim polymeric coating layer.
5. the method for the slim polymeric coating layer thickness of accurate test according to claim 4, is characterized in that described solvent is alcohol or distilled water.
6. the method for the slim polymeric coating layer thickness of accurate test according to claim 1, before it is characterized in that preparing polymeric coating layer on described sample stage, first surface preparation or covering are carried out in the area region of described sample stage, reduce the bond strength of this region polymeric coating layer and sample stage.
7. the method for the slim polymeric coating layer thickness of accurate test according to claim 6, is characterized in that referring in described surface preparation the area adopting silicone oil or adhesive sticker coated sample microscope carrier.
8. the method for the slim polymeric coating layer thickness of the accurate test according to claim 1 or 6, is characterized in that described area is at least 1/3 of the area of polymeric coating layer or sample stage.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105157643A (en) * | 2015-10-22 | 2015-12-16 | 廊坊立邦涂料有限公司 | Method for detecting polishing trace on painting surface |
| CN105603378A (en) * | 2016-01-05 | 2016-05-25 | 京东方科技集团股份有限公司 | Tool and method for measuring coating thickness of large-size substrate |
| CN110553616A (en) * | 2019-10-08 | 2019-12-10 | 江西洪都航空工业集团有限责任公司 | Method for measuring thickness of special-shaped surface coating |
| CN110715607A (en) * | 2019-10-10 | 2020-01-21 | 东莞市国瓷新材料科技有限公司 | Automatic measurement method for high-thermal-conductivity DPC ceramic substrate with thick copper plated on dry film |
| CN115265444A (en) * | 2022-09-26 | 2022-11-01 | 国标（北京）检验认证有限公司 | Method for measuring thickness of thin film sample by transmission electron microscope |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105157643A (en) * | 2015-10-22 | 2015-12-16 | 廊坊立邦涂料有限公司 | Method for detecting polishing trace on painting surface |
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| CN110715607A (en) * | 2019-10-10 | 2020-01-21 | 东莞市国瓷新材料科技有限公司 | Automatic measurement method for high-thermal-conductivity DPC ceramic substrate with thick copper plated on dry film |
| CN115265444A (en) * | 2022-09-26 | 2022-11-01 | 国标（北京）检验认证有限公司 | Method for measuring thickness of thin film sample by transmission electron microscope |
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Application publication date: 20150722 |