CN1924564A - Method for measuring several critical strain values of metal membrane in flexible substrate - Google Patents
Method for measuring several critical strain values of metal membrane in flexible substrate Download PDFInfo
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- CN1924564A CN1924564A CN 200610104580 CN200610104580A CN1924564A CN 1924564 A CN1924564 A CN 1924564A CN 200610104580 CN200610104580 CN 200610104580 CN 200610104580 A CN200610104580 A CN 200610104580A CN 1924564 A CN1924564 A CN 1924564A
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Abstract
This invention discloses one current load metal film stretching stress value test describing method, which comprises the following steps: processing current load and micro force stretching on the good metal film of interface; during this process recording the metal film stress curve and resistance change curve; acquiring the crack percentage stress curve through micro analysis by observing metal film. The current load metal film and flexible base board system invalid threshold system is composed of three threshold stress, such as the stress from resistance change to stress curve from linear phase to non-linear conversion; micro crack percentage stress curve back reducing as zero theory into threshold extension stress; resistance change to stress curve resistance runaway time into threshold crack unstable stress.
Description
Technical field
The present invention relates to the method for testing of the several critical strain values of metal membrane in the industries such as microelectronics, particularly method for measuring several critical strain values of metal membrane in flexible substrate.
Background technology
Flexible circuit board is widely used in VLSI (very large scale integrated circuit) and the microelectromechanical systems (MEMS), and generally the metallic film material (as Cu and Al) that connects up as metallization promptly is deposited on and forms metallic film/flexible base, board system on this flexible base, board.As engineering metal construction membraneous material, its plasticity or critical breaking strain are important index very, can be used for material safety design and life prediction.For the free metal film or be deposited on metallic film on the rigid substrates, therefore the normally fracture rapidly after local buckling and the unstability of its tensile properties is easy to directly determine its critical breaking strain from stress-strain curve.And for the metallic film that is deposited on the flexible base, board, because metallic film tends to stretch with the flexible base, board coupling in drawing process, metallic film often shows a kind of uniform plastic yield mode, yet keeps enough deformabilities even produced microscopic damage.From the angle analysis of microcosmic be exactly, though produced numerous tiny micro-cracks in the metallic film, but, the big crackle of film breaks do not occur being enough to cause, so film can continue to take place plastic yield to reach high tensile strain because these micro-cracks are equally distributed.
Although angle from the structural damage tolerance limit, metallic film has great tensile strain in metallic film/flexible base, board system, but owing to produced numerous micro-cracks already in the metallic film, the electric property that these micro-cracks will have a strong impact on metallic film is resistance for example, cause seriously shorten the actual life of metallic film, be significantly less than with the bimetry of maximum tension strain as critical indicator.Therefore, press for and set up a kind of new metallic film inefficacy critical strain and determine method, be beneficial to the material design reference.All the time, this problem has all been given great concern both at home and abroad, but relevant concrete definite method had not seen also but that report was arranged.
Summary of the invention
The objective of the invention is to overcome above-mentioned prior art deficiency, a kind of method for measuring several critical strain values of metal membrane in flexible substrate is provided, this method is simple, accurate and have apriority, is to realize the quantitatively advantageous methods of prevention of metallic film inefficacy.
Because the quantity of underbead crack and distribution can reflect by the resistance variations of material in the metal material, therefore in metallic film/flexible base, board system is stretched loading and record resistance variations-strain curve, the microstructure of observing metallic film in the drawing process by optical microscope or flying-spot microscope continuously changes, determine micro-crack percentage, draw the change curve of micro-crack percentage, determine critical strain by the unique point on this curve and the resistance variations-strain curve with strain.
Technical scheme of the present invention is achieved in that according to the following steps carries out:
(1) adopt the magnetron sputtering deposition method with deposit metal films on the polyimide flexible base, board, its elastic strain 〉=2%; Thickness of metal film 200 nanometers-20 micron; Deposition process parameters is: sputtering power 120-180W; Sputtering bias-voltage-60--80V; Background air pressure 3.0 * 10
-3-4.5 * 10
-3Pa; Operating air pressure Ar 0.1-0.3Pa;
(2) adopting range is stress σ-strain stress curve that little puller system of 250N is measured metallic film in metallic film/flexible base, board system, adopts resistance test measuring apparatus metal thin film resistor to change variation with strain stress in the drawing process, Δ=(R-R relatively
0)/R
0, R wherein
0Be the resistance value of metallic film before stretching, R is the resistance value of metallic film in the drawing process; Promptly obtain ε
iAnd ε
c
(3) the micro-crack percentage of observing metallic film in the drawing process continuously by flying-spot microscope changes, and draws the change curve of micro-crack percentage f with strain stress; Promptly obtain ε
p
Wherein, resistance variations on resistance variations-strain variation curve is defined as critical crack germinating strain stress from linear stage to the strain of nonlinear phase changing moment
iThe anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack expansion strain stress
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
c
The present invention has defined the inefficacy critical strain of metallic film first, to be used for the critical conditions under the quantitative measurement metallic film homogeneous deformation condition.The present invention can simulate the damage and the fracture of metallic film in actual condition metal membrane/flexible base, board system artificially, can be used for metallic film damage and the prediction of fracture and strick precaution in advance in the commercial Application, reduces the generation of the sudden failure phenomenon of device.
Embodiment
Below in conjunction with embodiment content of the present invention is described in further detail.
Embodiment 1:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 200 nanometers to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 150W; Sputtering bias-voltage-80V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 0.1Pa.Adopting range is the stress σ-strain stress curve of little puller system stretching metallic film/flexible base, board system mensuration metallic film of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=3.7%; ε
p=3.8%; ε
c=5.6%.
Embodiment 2:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 1.2 microns to the employing magnetron sputtering technique with metal A l thin film deposition, and deposition process parameters is: sputtering power 200W; Sputtering bias-voltage-70V; Background air pressure 3.0 * 10
-3Pa; Operating air pressure (Ar) 0.2Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=2.8%; ε
p=3.0%; ε
c=4.5%.
Embodiment 3:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 2.5 microns to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 120W; Sputtering bias-voltage-80V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 0.1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=2.55%; ε
p=2.7%; ε
c=3.6%.
Embodiment 4:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 10 microns to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 150W; Sputtering bias-voltage-60V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=2.3%; ε
p=2.4%; ε
c=3.1%.
Embodiment 5:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 15 microns to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 150W; Sputtering bias-voltage-80V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=2.0%; ε
p=2.1%; ε
c=3.0%.
Embodiment 6:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 20 microns to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 180W; Sputtering bias-voltage-80V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=1.75%; ε
p=1.9%; ε
c=2.6%.
Embodiment 7:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 25 microns to the employing magnetron sputtering technique with metal Cu thin film deposition, and deposition process parameters is: sputtering power 130W; Sputtering bias-voltage-60V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=1.4%; ε
p=1.5%; ε
c=2.1%.
Embodiment 8:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 25 microns to the employing magnetron sputtering technique with metal A l thin film deposition, and deposition process parameters is: sputtering power 130W; Sputtering bias-voltage-60V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=1.1%; ε
p=1.2%; ε
c=1.9%.
Embodiment 9:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 25 microns to the employing magnetron sputtering technique with metal A g thin film deposition, and deposition process parameters is: sputtering power 130W; Sputtering bias-voltage-60V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=1.7%; ε
p=1.8%; ε
c=2.5%.
Embodiment 10:
The polyimide flexible base, board is processed into traditional tensile sample shape, and (20 * 6mm) is the effective workspace of sample, and the roomy district at two ends is the stretching clamp area in middle long narrow district.On effective workspace, film thickness is 25 microns to the employing magnetron sputtering technique with metal Fe thin film deposition, and deposition process parameters is: sputtering power 130W; Sputtering bias-voltage-60V; Background air pressure 4.5 * 10
-3Pa; Operating air pressure (Ar) 1Pa.Adopting range is little puller system stretching metallic film/flexible base, board system of 250N, adopts the variation of the relative changes delta of resistance test measuring apparatus metal thin film resistor with strain stress in the drawing process; The microstructure of observing metallic film in the drawing process by flying-spot microscope continuously changes, and draws micro-crack percentage f-strain stress curve.The anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack germinating strain stress
iResistance variations on resistance variations-strain curve is defined as critical crack expansion strain stress from linear stage to the strain of nonlinear phase changing moment
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
cDetermine ε respectively by measuring curve
i=1.2%; ε
p=1.3%; ε
c=2.0%.
Claims (1)
1, the method for testing of several critical strain values of metal membrane in flexible substrate is characterized in that, may further comprise the steps:
(1) adopt the magnetron sputtering deposition method with deposit metal films on the polyimide flexible base, board, its elastic strain 〉=2%; Thickness of metal film 200 nanometers-20 micron; Deposition process parameters is: sputtering power 120-180W; Sputtering bias-voltage-60--80V; Background air pressure 3.0 * 10
-3-4.5 * 10
-3Pa; Operating air pressure Ar 0.1-0.3Pa;
(2) adopting range is stress σ-strain stress curve that little puller system of 250N is measured metallic film in metallic film/flexible base, board system, adopts resistance test measuring apparatus metal thin film resistor to change variation with strain stress in the drawing process, Δ=(R-R relatively
0)/R
0, R wherein
0Be the resistance value of metallic film before stretching, R is the resistance value of metallic film in the drawing process; Promptly obtain ε
iAnd ε
c
(3) the micro-crack percentage of observing metallic film in the drawing process continuously by flying-spot microscope changes, and draws the change curve of micro-crack percentage f with strain stress; Promptly obtain ε
p
Wherein, resistance variations on resistance variations-strain variation curve is defined as critical crack germinating strain stress from linear stage to the strain of nonlinear phase changing moment
iThe anti-theoretical strain that pushes away when being zero of micro-crack percentage in micro-crack percentage-strain curve is defined as critical crack expansion strain stress
pSharp increase strain is constantly taken place in resistance on resistance variations-strain curve be defined as critical crack unstability strain stress
c
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|---|---|---|---|
| CNB2006101045804A CN100561210C (en) | 2006-09-15 | 2006-09-15 | Method for measuring several critical strain values of metal membrane in flexible substrate |
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|---|---|---|---|
| CNB2006101045804A CN100561210C (en) | 2006-09-15 | 2006-09-15 | Method for measuring several critical strain values of metal membrane in flexible substrate |
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|---|---|
| CN1924564A true CN1924564A (en) | 2007-03-07 |
| CN100561210C CN100561210C (en) | 2009-11-18 |
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|---|---|---|---|
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101226163B (en) * | 2008-01-22 | 2010-11-10 | 西安交通大学 | Method for measuring metallic film fatigue life on a flexible substrate |
| CN105082662A (en) * | 2015-07-27 | 2015-11-25 | 河南科技大学 | Method for reducing crack generation on high-melting metal film on flexible matrix |
| CN105140141A (en) * | 2015-07-27 | 2015-12-09 | 河南科技大学 | Method for restraining hillocks formation on copper alloy thin film surface by applying prestressing force |
| CN105424721A (en) * | 2015-12-11 | 2016-03-23 | 南京神源生智能科技有限公司 | Metal strain gauge defect automatic detection system |
| CN109883314A (en) * | 2019-03-08 | 2019-06-14 | 吉林大学 | A kind of fexible film sensing element sensibility testing arrangement and its method |
| CN110082207A (en) * | 2019-05-05 | 2019-08-02 | 中国人民解放军陆军装甲兵学院 | Detect method and apparatus, system and the storage medium of coating material strain failure |
| CN111351702A (en) * | 2020-03-19 | 2020-06-30 | 中国科学院金属研究所 | Method for determining fracture strain of flexible substrate metal film |
| WO2022247018A1 (en) * | 2021-05-26 | 2022-12-01 | 苏州大学 | Microcrack strain sensing element, preparation method therefor and application thereof |
-
2006
- 2006-09-15 CN CNB2006101045804A patent/CN100561210C/en not_active Expired - Fee Related
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101226163B (en) * | 2008-01-22 | 2010-11-10 | 西安交通大学 | Method for measuring metallic film fatigue life on a flexible substrate |
| CN105082662A (en) * | 2015-07-27 | 2015-11-25 | 河南科技大学 | Method for reducing crack generation on high-melting metal film on flexible matrix |
| CN105140141A (en) * | 2015-07-27 | 2015-12-09 | 河南科技大学 | Method for restraining hillocks formation on copper alloy thin film surface by applying prestressing force |
| CN105082662B (en) * | 2015-07-27 | 2018-01-02 | 河南科技大学 | A kind of method that high melting point metal film cracks on reduction flexible substrate |
| CN105140141B (en) * | 2015-07-27 | 2018-01-26 | 河南科技大学 | A kind of prestressing force that applies suppresses the convex method in copper alloy thin films surface formation mound |
| CN105424721A (en) * | 2015-12-11 | 2016-03-23 | 南京神源生智能科技有限公司 | Metal strain gauge defect automatic detection system |
| CN105424721B (en) * | 2015-12-11 | 2018-07-13 | 南京神源生智能科技有限公司 | A kind of metal strain meter defect automatic checkout system |
| CN109883314A (en) * | 2019-03-08 | 2019-06-14 | 吉林大学 | A kind of fexible film sensing element sensibility testing arrangement and its method |
| CN110082207A (en) * | 2019-05-05 | 2019-08-02 | 中国人民解放军陆军装甲兵学院 | Detect method and apparatus, system and the storage medium of coating material strain failure |
| CN111351702A (en) * | 2020-03-19 | 2020-06-30 | 中国科学院金属研究所 | Method for determining fracture strain of flexible substrate metal film |
| CN111351702B (en) * | 2020-03-19 | 2021-10-15 | 中国科学院金属研究所 | Method for determining fracture strain of flexible substrate metal film |
| WO2022247018A1 (en) * | 2021-05-26 | 2022-12-01 | 苏州大学 | Microcrack strain sensing element, preparation method therefor and application thereof |
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Effective date of registration: 20160414 Address after: 276017 Shandong city of Linyi province high tech Zone bimonthly Road Technology Park D block floor West Fourth Patentee after: Shandong Hechuang Coating Technology Co. Ltd. Address before: 710049 Xianning Road, Shaanxi, China, No. 28, No. Patentee before: Xi'an Jiaotong University |
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Granted publication date: 20091118 Termination date: 20190915 |