CN103398662A - Method and device for measuring thickness of 10 to 100 Mum solid thin films - Google Patents
Method and device for measuring thickness of 10 to 100 Mum solid thin films Download PDFInfo
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- CN103398662A CN103398662A CN2013103439764A CN201310343976A CN103398662A CN 103398662 A CN103398662 A CN 103398662A CN 2013103439764 A CN2013103439764 A CN 2013103439764A CN 201310343976 A CN201310343976 A CN 201310343976A CN 103398662 A CN103398662 A CN 103398662A
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Abstract
The invention discloses a method and device for measuring the thickness of 10 to 100 Mum solid thin films. Two alumina ceramic clamping pieces clamp a naked thin film or a thin film coated on a substrate; the alumina ceramic clamping pieces, which are clamped by fixtures, are fixed through a relay or an RbFeB magnet, and are placed under the microscope of a Vickers hardness scale for observation; the alumina ceramic clamping pieces are placed vertically. As contrast difference exists between the thin film and each alumina ceramic clamping piece/the substrate, the micrometer head of the microscope can read out the distance between the two alumina ceramic clamping pieces or the distance between each of the alumina ceramic clamping pieces near two sides of the thin film and one side of the substrate, and the distance is the thickness of the thin film. As the micrometer head of the microscope is used for reading out directly, the accuracy is high, the operation is simple, and the measuring accuracy can be 0.5 to 1 Mum. The method is simple; the device is easy to operate; the precision is high; the method and the device can be used in not only industry but also laboratories.
Description
Technical field
The present invention relates to a kind of method of measuring solid film, be specifically related to measuring method and the device of 10～100 μ m solid film thickness.
Background technology
The film of industry or laboratory applications, its thickness are very important parameters." size effect " of film has influence on the character such as film resiativity, Hall coefficient, light reflectivity, and can be related to film work.
The measuring method of common 10～100 μ m film thicknesses has the optical meanss such as light transmission, interference, polarization, reflectometry, but for solid film, the method is inapplicable; X-ray thickness gauge, but scanning electron microscope, step instrument, holography method testing film thickness and precision are high expensive, operate comparatively loaded down with trivial details; Supersonic thickness meter, eddy current thickness meter etc. need standard sample, increase and measure cost, and the instrument cost is higher.But expensive, method of testing bothers, and ordinary light source can't meet the thickness measuring condition of light absorbent.
For 10～100 μ m solid films, particularly be attached to the measured film thickness of substrate, need especially a kind of simple to operate, low cost, the higher measuring method of accuracy.
Summary of the invention
The objective of the invention is, for overcoming above-mentioned the deficiencies in the prior art, provides measuring method and the device of 10～100 μ m solid film thickness.
For achieving the above object, the present invention adopts following technical proposals:
the measuring method of 10～100 μ m solid film thickness, utilize two piece aluminum oxide pottery intermediate plates to clamp exposed film or be coated on suprabasil film, with relay or the fixing aluminium oxide ceramics intermediate plate with the fixture clamping of nd-fe-b magnet, and be placed in the scleroscopic micro-Microscopic observation of dimension formula, the aluminium oxide ceramics intermediate plate is vertically placed, between described film and aluminium oxide ceramics intermediate plate or substrate, there is contrast difference, utilize microscopical differential head to read distance or the aluminium oxide ceramics intermediate plate of close film both sides and the distance between substrate one side between two piece aluminum oxide pottery intermediate plates, be film thickness.
Described film is ferrous acid lanthanum film, lanthanum manganate film, Lanthanum Chromite film, LiMn2O4 film or PVC film, with the aluminium oxide ceramics intermediate plate, contrast difference is arranged under the microscope, as long as the interface that can find out aluminium oxide just can Thickness Measurement by Microwave; Described substrate is the non-blacks such as aluminium oxide, aluminium foil or silicon dioxide, and is strong to the reflection of light effect, with film, forms contrast difference, examine under a microscope and can observe pattern, or reflective bright district.
The size of described film is less than or equal to 25mm * 50mm.
Described substrate has a flat side, and this flat side contacts with film, and concordant with a slice aluminium oxide ceramics intermediate plate wherein.
Described microscopic fields of view has 100 and 400 times, and wherein, during with 100 times of visual field test, net result is 4 times of baseline results.
Described film thickness is shape thickness, is the average thickness of film; When film was clamped in two piece aluminum oxides potteries intermediate plates middle, two sides of film directly contacted with the aluminium oxide ceramics intermediate plate, and the shape thickness of film is actual thickness.
The measurement mechanism of 10～100 μ m solid film thickness, comprise two piece aluminum oxide pottery intermediate plates by the fixture clamping, between described two piece aluminum oxide pottery intermediate plates, accompany exposed film or be coated on suprabasil film, between described film and aluminium oxide ceramics intermediate plate or substrate, have contrast difference.
The both sides of described two piece aluminum oxide pottery intermediate plates are fixed by relay or nd-fe-b magnet.
Described film is ferrous acid lanthanum film, lanthanum manganate film, Lanthanum Chromite film, LiMn2O4 film or PVC film, and the size of described film is less than or equal to 25mm * 50mm.
Described substrate is aluminium oxide, aluminium foil or silicon dioxide, and described substrate has a flat side, and this flat side contacts with film, and concordant with a slice aluminium oxide ceramics intermediate plate wherein.Principle of work of the present invention:
Film is extinction, present black, and the aluminium oxide ceramics intermediate plate is white, and aluminium oxide ceramics intermediate plate of the present invention border is straight, and corner angle are clearly demarcated, with the contrast of solid film material, differ greatly, with respect to solid film, the microstructure of aluminium oxide ceramics intermediate plate after 100 optical amplifiers be clear, be easy to differentiate, as Fig. 4, utilize microscopical differential head can read the distance between two piece aluminum oxide pottery intermediate plates, be film thickness.
Film is difficult for observing interface under the microscope, and the aluminium oxide ceramics intermediate plate can be observed border clearly, aluminium oxide ceramics intermediate plate of the present invention border is straight, corner angle are clearly demarcated, with the contrast of membraneous material, differ greatly, with respect to film, the microstructure of aluminium oxide ceramics intermediate plate after 100 optical amplifiers be clear, be easy to differentiate, as Fig. 2, utilize microscopical differential head can read the distance between two piece aluminum oxide pottery intermediate plates, be film thickness.And for the film that substrate is arranged, if base material also can be told the contact interface with film under the microscope clearly, the distance between this interface and alumina ceramic plate is film thickness so, as shown in Figure 4.
Aluminium oxide ceramics intermediate plate of the present invention is vertically placed.Thickness measuring is not subjected to the impact of film shape, and the test surfaces of film tilts or out-of-flatness affects the test nothing; But for being coated on suprabasil film, substrate should have a flat side, and concordant with intermediate plate.
The film thickness of the present invention's test is the shape thickness of film, is the average thickness of film sample.As shown in Figure 3, film is clamped in the middle of the aluminium oxide ceramics intermediate plate, and two sides of film directly contact with the aluminium oxide ceramics intermediate plate, are similar to the interface of coincidence, and the distance between the aluminium oxide ceramics intermediate plate namely equals film thickness like this.
The invention has the beneficial effects as follows, the present invention utilizes the direct reading of the microscopical differential head of dimension formula sclerometer, accuracy is high, simple to operate, the precision that its measuring accuracy can arrive 0.5～1 μ m(differential head is 0.01 μ m, actual the roughness of alumina wafer is 0.40～0.42 μ m when the test of film, and thickness and precision is between 0.5～1 μ m).The present invention is simple for the solid film thickness measuring method, installs easy to operately, and degree of accuracy is high, but but both industrial application also use in laboratory.
The accompanying drawing explanation
Fig. 1 is the measurement mechanism figure of film, (a) front view (b) left view (c) vertical view;
Fig. 2 is the microstructure figure of aluminium oxide ceramics intermediate plate after amplifying under 100 optical microscopes;
Fig. 3 is the measurement mechanism vertical view that is coated on suprabasil film;
Fig. 4 is the scanning electron microscope (SEM) photograph of thickness measure;
1. aluminium oxide ceramics intermediate plates wherein, 2. exposed film, 3. relay or nd-fe-b magnet, 4. be coated on suprabasil film, 5. substrate, 6. fixture.
Embodiment
The present invention will be further elaborated below in conjunction with drawings and Examples, should be noted that following explanation is only in order to explain the present invention, does not limit its content.
Embodiment 1:
Measurement mechanism of the present invention, comprise between two piece aluminum oxide pottery intermediate plate 1, two piece aluminum oxide pottery intermediate plates 1 by fixture 6 clampings and accompany exposed film 2.The both sides of two piece aluminum oxide pottery intermediate plates 1 are fixing by relay or nd-fe-b magnet 3.
The measuring method of 10～100 μ m solid film thickness, as shown in Figure 1, utilize two piece aluminum oxide pottery intermediate plates 1 to clamp PVC film (being film 2 exposed in Fig. 1 (a)), and exposed film 2 is of a size of 10mm * 10mm.With the fixing aluminium oxide ceramics intermediate plate 1 with fixture 6 clampings of relay, and be placed in the scleroscopic 400 times of optical microphotograph Microscopic observations of HV-100 dimension formula, aluminium oxide ceramics intermediate plate 1 is vertically placed, due to exposed film 2 and aluminium oxide ceramics intermediate plate 1 contrast difference, utilize microscopical differential head to read the distance between two aluminium oxide ceramics intermediate plates 1, be film thickness.Read 4 secondary data and then average, data are as shown in table 1.
Table 1
| Number of |
1 | 2 | 3 | 4 | Mean value | Variance |
| Thickness/μ m | 61.08 | 60.04 | 61.32 | 59.92 | 60.55 | 0.39 |
Above-mentioned PVC film is measured to its thickness with micrometer caliper, and test result is as shown in table 2.
Table 2
| Number of |
1 | 2 | 3 | 4 | Mean value | Variance |
| Thickness/μ m | 60 | 61 | 62 | 59 | 60.5 | 1.67 |
Embodiment 2:
Measurement mechanism of the present invention, comprise between two piece aluminum oxide pottery intermediate plate 1, two piece aluminum oxide pottery intermediate plates 1 by fixture 6 clampings and accompany and be coated on suprabasil film 4.The both sides of two piece aluminum oxide pottery intermediate plates 1 are fixing by relay or nd-fe-b magnet 3.
The measuring method of 10～100 μ m solid film thickness, as shown in Figure 3, that utilizes two piece aluminum oxides potteries intermediate plates 1 to clamp to apply on alumina substrate 2 mixes strontium ferrous acid lanthanum film (being the suprabasil film 4 that is coated in Fig. 3), is coated on suprabasil film 4 and is of a size of 10mm * 10mm.With the fixing aluminium oxide ceramics intermediate plate 1 with fixture 6 clampings of nd-fe-b magnet, and be placed in the scleroscopic 100 times of optical microphotograph Microscopic observations of HV-100 dimension formula, wherein the metallographic pattern of aluminium oxide as shown in Figure 2.Aluminium oxide ceramics intermediate plate 1 is vertically placed, due to the contrast difference that is coated between suprabasil film 4 and aluminium oxide ceramics intermediate plate 1 and substrate 5, utilize microscopical differential head to read near being coated on the aluminium oxide ceramics intermediate plate 1 of suprabasil film 4 both sides and the distance between substrate 5 one sides, multiply by 4 and be film thickness.Read 4 secondary data and then average, data are as shown in table 3.
Table 3
| Number of |
1 | 2 | 3 | 4 | Mean value | Variance |
| Thickness/μ m | 63.00 | 62.16 | 59.40 | 59.92 | 60.7 | 2.8 |
And with JEOLJSM-6380LA sweep electron microscopic measure thickness detailed process be: sample thickness face metal spraying is observed sample thickness face clearly after processing under scanning electron microscope, photographic images then, as shown in Figure 4.The thickness of three point measurement films in survey sheet (A in Fig. 4, B, C), get the mean value of measuring for three times
, then the length of surveying 20 μ m scales is the D in 15.88(such as Fig. 4), the recycling formula
Calculate the thickness of film, what draw the results are shown in Table shown in 4.
Table 4
Although above-mentionedly by reference to the accompanying drawings the specific embodiment of the present invention is described; but be not limiting the scope of the invention; on the basis of technical scheme of the present invention, those skilled in the art do not need to pay various modifications that creative work can make or distortion still in protection scope of the present invention.
Claims (10)
1.10 the measuring method of～100 μ m solid film thickness, it is characterized in that, utilize two piece aluminum oxide pottery intermediate plates to clamp exposed film or be coated on suprabasil film, with relay or the fixing aluminium oxide ceramics intermediate plate with the fixture clamping of nd-fe-b magnet, and be placed in the scleroscopic micro-Microscopic observation of dimension formula, the aluminium oxide ceramics intermediate plate is vertically placed, between described film and aluminium oxide ceramics intermediate plate or substrate, there is contrast difference, utilize microscopical differential head to read distance or the aluminium oxide ceramics intermediate plate of close film both sides and the distance between substrate one side between two piece aluminum oxide pottery intermediate plates, be film thickness.
2. measuring method according to claim 1, is characterized in that, described film is ferrous acid lanthanum film, lanthanum manganate film, Lanthanum Chromite film, LiMn2O4 film or PVC film; Described substrate is aluminium oxide, aluminium foil or silicon dioxide.
3. measuring method according to claim 1, is characterized in that, the size of described film is less than or equal to 25mm * 50mm.
4. measuring method according to claim 1, is characterized in that, described substrate has a flat side, and this flat side contacts with film, and concordant with a slice aluminium oxide ceramics intermediate plate wherein.
5. measuring method according to claim 1, is characterized in that, described microscope is 100 times of optical microscopes.
6. measuring method according to claim 1, is characterized in that, described film thickness is shape thickness, is the average thickness of film; When film was clamped in two piece aluminum oxides potteries intermediate plates middle, two sides of film directly contacted with the aluminium oxide ceramics intermediate plate, and the shape thickness of film is actual thickness.
7.10 the measurement mechanism of～100 μ m solid film thickness, it is characterized in that, comprise two piece aluminum oxide pottery intermediate plates by the fixture clamping, between described two piece aluminum oxide pottery intermediate plates, accompany exposed film or be coated on suprabasil film, between described film and aluminium oxide ceramics intermediate plate or substrate, have contrast difference.
8. measurement mechanism according to claim 7, is characterized in that, the both sides of described two piece aluminum oxide pottery intermediate plates are fixed by relay or nd-fe-b magnet.
9. measurement mechanism according to claim 7, is characterized in that, described film is ferrous acid lanthanum film, lanthanum manganate film, Lanthanum Chromite film, LiMn2O4 film or PVC film, and the size of described film is less than or equal to 25mm * 50mm.
10. measurement mechanism according to claim 7, is characterized in that, described substrate is aluminium oxide, aluminium foil or silicon dioxide, and described substrate has a flat side, and this flat side contacts with film, and concordant with a slice aluminium oxide ceramics intermediate plate wherein.
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Cited By (3)
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| CN106370115A (en) * | 2016-08-26 | 2017-02-01 | 上海紫江新材料科技有限公司 | Aluminum-plastic film aluminum layer thickness detection method |
| CN108895971A (en) * | 2018-07-05 | 2018-11-27 | 北京科技大学 | A kind of high-precision control thin liquid film thickness forms device and application method |
| CN112194507A (en) * | 2020-09-21 | 2021-01-08 | 江苏大学 | High-temperature thermal shock resistant wide-spectrum high-absorption photo-thermal coating and preparation method thereof |
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| CN108895971A (en) * | 2018-07-05 | 2018-11-27 | 北京科技大学 | A kind of high-precision control thin liquid film thickness forms device and application method |
| CN108895971B (en) * | 2018-07-05 | 2024-01-23 | 北京科技大学 | High-precision thin liquid film thickness control forming device and using method |
| CN112194507A (en) * | 2020-09-21 | 2021-01-08 | 江苏大学 | High-temperature thermal shock resistant wide-spectrum high-absorption photo-thermal coating and preparation method thereof |
| CN112194507B (en) * | 2020-09-21 | 2022-02-15 | 江苏大学 | High-temperature thermal shock resistant wide-spectrum high-absorption photo-thermal coating and preparation method thereof |
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