CN106248276B - A method of measurement metal micro structure residual stress - Google Patents
A method of measurement metal micro structure residual stress Download PDFInfo
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- CN106248276B CN106248276B CN201610538415.3A CN201610538415A CN106248276B CN 106248276 B CN106248276 B CN 106248276B CN 201610538415 A CN201610538415 A CN 201610538415A CN 106248276 B CN106248276 B CN 106248276B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L5/00—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes
- G01L5/0047—Apparatus for, or methods of, measuring force, work, mechanical power, or torque, specially adapted for specific purposes measuring forces due to residual stresses
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Abstract
A method of measurement metal micro structure residual stress belongs to micro-fabrication technology field, is related to the measurement method of metal micro structure residual stress.Solid particle with Raman active is pre-processed, suspension is mixed to form with electroforming solution and carries out micro- electroforming.Using solid particle as stress trace signals, the residual stress measurement of metal micro structure is carried out by micro-Raman spectroscopy technique.By addition there is the solid particle of Raman active and metal to carry out co-deposition and prepares metal micro structure, solves the limitation that X-ray diffraction method is unable to measure metal micro structure residual stress, and expand application range of the micro-Raman spectroscopy technique in terms of measuring residual stress, have the characteristics that have a wide range of application, simply, efficiently, to improve the dimensional accuracy and production yield rate of metal microdevices.
Description
Technical field
The invention belongs to micro-fabrication technology fields, are related to a kind of method for measuring metal micro structure residual stress.
Background technique
In technical process using micro- galvanoplastics production metal microdevices, inevitably resulted from micro- electroformed layer
Residual stress.Biggish residual stress is easy that micro element is made face crack, malformation, whole the problems such as falling off, this pole occur
The earth reduces the yield rate and service life of micro-devices fabrication.
Generally there is MEMS metal microdevices functional structure to design, and minimum feature size is in micron dimension.Currently,
Most common metal deposition layer residual stress measuring method is X-ray diffraction method.But this method can only be used to measurement structure size
Sample greater than 10mm × 10mm, and X-ray diffraction method is influenced that positioning measurement can not be carried out by light beam precision, can not achieve
The distribution of micro-structure residual stress is studied.With the raising of light beam precision and positioning system, micro-Raman spectroscopy technique relies on
Non-contact nondestructive wound, spatial resolution high (laser facula as low as 1um), measurement accuracy height obtain in terms of residual stress measurement
Using.Magazine Optics and Lasers in Engineering2005, volume 43, the 8th phase, utilized by the 847-855 pages
Micro- Raman spectroscopy measure prepared on a silicon substrate with electrochemical erosion method generated in porous silicon film technical process it is residual
Residue stress, the residual stress size and porous silicon film that compared corrosion region and non-corrosion region are answered with silicon base interface remnants
Power distribution situation.Magazine China Mechanical Engineering 2005, volume 16, the 14th phase, utilized micro- Raman spectrum by the 1292-1295 pages
Technology carries out residual stress distribution test to the micro cantilever structure of the eight beams support formed under standard body silicon etching process,
The normalized Raman characteristic peak of middle silicon is 520cm-1.Magazine Microelectronics Journal2007, volume 38, the 1st phase,
Also the residual stress of silicon micro cantilever structure is measured in the 87-90 pages using micro-Raman spectroscopy technique.
In the research of micro- Raman spectroscopy measurement micro-structure residual stress utilized above, the crystal structure of institute's research object
There is molecular link.However, metal is atomic structure, do not have vibration and rotational freedom, metal surface electronics and atomic kernel
The plasma that border is constituted has strong absorption to laser, so that it can not interact with interior atoms, theoretically micro- Raman
Spectroscopic methodology is not capable of measuring the residual stress of metal microdevices.But the spatial high resolution of micro- Raman spectroscopy, directly measurement are answered
The features such as power, has unique advantage to analysis micro-structure residual stress distribution.Therefore, one is established by micro- Raman spectroscopy
The method that kind can carry out residual stress measurement to metal micro structure has important application value.
Summary of the invention
In view of the problems of the existing technology the present invention, provides a kind of method for measuring metal micro structure residual stress,
Solid particle with Raman active is pre-processed, suspension is mixed to form with electroforming solution and carries out micro- electroforming.By solid
Grain is used as stress trace signals, and the residual stress measurement of metal micro structure is carried out by micro-Raman spectroscopy technique.
The specific technical solution of the present invention is as follows:
A method of measurement metal micro structure residual stress, detailed making step are as follows:
Step 1 pre-processes the solid particle with Raman active
Suspended carbon, greasy dirt, the oxide impurity for cleaning solid particle removal surface, obtain the solid particle of clean surface.
Step 2 makes electroforming suspension
The solid particle of clean surface is mixed into wetting with surfactant, and applies ultrasonic diffusion；Heating electroforming solution arrives
Electroforming temperature is simultaneously kept the temperature using heating water bath；It will be poured slowly into electroforming solution by the solid particle solution of ultrasound diffusion,
And it carries out magnetic agitation 2-4h and forms the electroforming suspension being evenly distributed.
Step 3, micro- electroforming
Firstly, making photoresist based on UV-LIGA technique, carrying out uv-exposure using mask plate and developing, electroforming is obtained
Micro-structure glue film；Then micro- electroforming is carried out in the electroforming tank equipped with electroforming suspension.Formulation of electroforming solution: nickel sulfamic acid 595-
605g/L, nickel chloride 4-6g/L, boric acid 30-40g/L.Electroforming solution pH value is 3.8~4.0, and electroforming temperature is 45-50 DEG C, electric current
Density is 1-3A/dm2.Solid grain size is 2-7um, content 10-30g/L.Obtaining outer dimension is millimeter magnitude, micro- knot
Metal micro structure of the structure minimum feature size within the scope of 15-25um.
Step 4, micro- Raman spectrum test
It chooses silicon wafer and carries out micro- Raman Measurement, standard frequency of the obtained raman frequency as calibrating instrument error；To step
A rapid pretreated solid particle carries out micro- Raman spectrum test, obtains the Raman signatures frequency under solid particle unstress state
Rate ω0；Micro- Raman spectrum test is carried out to the solid particle in step 3 metal micro structure cast layer, solid particle is obtained and is answering
Raman signatures frequencies omega under power state1；According to formula
(1) metal micro structure residual-stress value σ is calculated；Wherein, K is stress factor.
σ=K × (ω1-ω0) (1)
Effect and benefit of the invention: a kind of method for measuring metal micro structure residual stress is provided, is had by addition
There are the solid particle of Raman active and metal to carry out co-deposition and prepare metal micro structure, solves X-ray diffraction method and be unable to measure
The limitation of metal micro structure residual stress, and application range of the micro-Raman spectroscopy technique in terms of measuring residual stress is expanded,
Have the characteristics that have a wide range of application, simply, efficiently, to improve the dimensional accuracy and production yield rate of metal microdevices.
Detailed description of the invention
Fig. 1 metal micro structure mask plate schematic diagram
Fig. 2 .UV-LIGA process flow diagram
The micro- electroforming schematic diagram of Fig. 3
In figure: 1 metallic substrates；2 photoresists；3 mask plates；4 ultraviolet lights；5 micro-structure electroforming glue films；6 water baths；7 electroforming
Slot；8 electroforming suspension；9 magnetic rotors.
Specific embodiment
A specific embodiment of the invention is described in detail below in conjunction with technical solution and attached drawing.
Attached drawing 1 is the metal Microspring mask plate schematic diagram for photoetching, the micro-structure overall dimensions be 3.74mm ×
1.14mm, spring minimum feature are 25um.Based on attached UV-LIGA process flow shown in Fig. 2, metal micro structure electricity has been made
Cast glue film.The co-deposition of solid particle and metal micro structure is carried out in attached micro- electroforming apparatus shown in Fig. 3 later.A kind of measurement
The method of metal micro structure residual stress comprising steps are as follows:
(1) pretreatment has the solid particle of Raman active.It is fallen firstly, weighing the SiC solid particle that 20g partial size is 5um
Enter into 500ml beaker, cleans solid particle, the suspended carbon on filtering removal surface with deionized water；Secondly, being 20% with concentration
NaOH aqueous solution soaking 30s remove solid particles surface greasy dirt；Finally, impregnating 3h removal with the HCl solution that concentration is 18%
The oxide of solid particles surface；After HCl solution immersion, cleaning repeated flushing completely with deionized water prevents HCl solution residual
It stays.
(2) electroforming suspension is made
It is mixed firstly, weighing 0.4g surfactant with 100ml deionized water, is poured into cleaned SiC particulate
In, carry out ultrasound diffusion 30min, ultrasonic power 100W, frequency 40KHz；It is heated secondly, taking out 900ml electroforming solution
And keep the temperature, temperature is 50 DEG C；Finally, by being poured slowly into electroforming solution by the solid particle solution of ultrasound diffusion, and carry out
Magnetic agitation, magnetic agitation rotating speed 800rpm, time 4h.
(3) micro- electroforming
Select the beaker of 800ml as electroforming tank, anode and cathode spacing is 35mm.During electroforming, heat collecting type perseverance is utilized
Warm magnetic stirring apparatus carries out water-bath heat preservation to electroforming process and applies magnetic agitation, and electroforming temperature is 50 DEG C, magnetic agitation rotating speed
For 600rpm.Formulation of electroforming solution: nickel sulfamic acid 600g/L, nickel chloride 5g/L, boric acid 30g/L.Micro- electroformed nickel process conditions are as follows:
Casting liquid pH value is 4.0, current density 1A/dm2.SiC solid content is 20g/L.
(4) micro- Raman spectrum test
Firstly, choosing silicon wafer carries out micro- Raman spectrum test, it is accurately positioned and is swashed using 100 times of object lens amplifications when Raman is tested
Illumination is mapped to sample surfaces, optical maser wavelength 532nm, power 1mW, and grating scale is 1800 lines/nm, the raman characteristic peak of silicon
Frequency is 521cm-1；Secondly, taking out a small amount of cleaned SiC particulate carries out micro- Raman spectrum test, raman characteristic peak frequency
ω0For 792.98cm-1；Finally, micro- Raman spectrum test is carried out to the SiC particulate in metal micro structure cast layer, the SiC in cast layer
Particle raman characteristic peak frequencies omega1For 793.51cm-1,
σ=K × (ω1-ω0) (1)
The stress factor K of SiC solid particle be -434.78, using formula (1) obtain its residual-stress value σ be -
253.4MPa。
Claims (9)
1. a kind of method for measuring metal micro structure residual stress, which is characterized in that comprise the following steps that
Step 1 pre-processes the solid particle with Raman active: suspended carbon, greasy dirt, the oxygen on cleaning solid particle removal surface
Compound impurity obtains the solid particle of clean surface；
Step 2 makes electroforming suspension: the solid particle of clean surface being mixed wetting with surfactant, and applies ultrasound
Diffusion；Electroforming solution is heated to electroforming temperature；It will be poured slowly into electroforming solution, and carry out by the solid particle solution of ultrasound diffusion
Magnetic agitation 2-4h forms the electroforming suspension being evenly distributed；
Step 3, micro- electroforming: making photoresist based on UV-LIGA technique, carries out uv-exposure using mask plate and develops, obtains
Electric casting micro structure glue film；Then micro- electroforming is carried out in the electroforming tank equipped with electroforming suspension, and applies magnetic agitation；It obtains outer
Metal micro structure of the shape having a size of millimeter magnitude；
Micro- Raman spectrum test: step 4 chooses silicon wafer and carries out micro- Raman Measurement, obtained raman frequency is missed as calibrating instrument
The standard frequency of difference；Micro- Raman spectrum test is carried out to the pretreated solid particle of step 1, it is unstressed to obtain solid particle
Raman signatures frequencies omega under state0；Micro- Raman spectrum test is carried out to the solid particle in step 3 metal micro structure cast layer,
Obtain Raman signatures frequencies omega of the solid particle in the case where there is stress state1；Metal micro structure remnants are calculated according to formula (1)
Stress value σ；Wherein, K is stress factor
σ=K × (ω1-ω0) (1)。
2. a kind of method for measuring metal micro structure residual stress according to claim 1, which is characterized in that described
Solid grain size with Raman active is 2~7um.
3. according to claim 1 or a kind of method of measurement metal micro structure residual stress described in 2, which is characterized in that gold
Belong to the minimum feature size of micro-structure within the scope of 10~25um.
4. according to claim 1 or a kind of method of measurement metal micro structure residual stress described in 2, which is characterized in that step
Micro- Raman spectrum test parameter in rapid four: grating scale is not less than 1800 lines/nm.
5. a kind of method for measuring metal micro structure residual stress according to claim 3, which is characterized in that step 4
In micro- Raman spectrum test parameter: grating scale be not less than 1800 lines/nm.
6. a kind of method of measurement metal micro structure residual stress described according to claim 1 or 2 or 5, which is characterized in that
Solid particle described in step 1 with Raman active is silicon carbide, aluminium oxide, boron carbide or cerium oxide.
7. a kind of method for measuring metal micro structure residual stress according to claim 3, which is characterized in that step 1
Described in the solid particle with Raman active be silicon carbide, aluminium oxide, boron carbide or cerium oxide.
8. a kind of method for measuring metal micro structure residual stress according to claim 4, which is characterized in that step 1
Described in the solid particle with Raman active be silicon carbide, aluminium oxide, boron carbide or cerium oxide.
9. a kind of method of measurement metal micro structure residual stress described according to claim 1 or 2 or 5 or 7 or 8, special
Sign is, the formulation of electroforming solution are as follows: 595~605g/L of nickel sulfamic acid, 4~6g/L of nickel chloride, 30~40g/L of boric acid；
Micro- electroformed nickel process conditions are as follows: pH value 3.8~4.0, temperature 45 C~50 DEG C, 1~3A/dm of current density2。
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| CN110579298A (en) * | 2019-10-21 | 2019-12-17 | 中南大学 | high-precision electroforming stress online detection method based on thermal balance condition |
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| US5898302A (en) * | 1997-11-25 | 1999-04-27 | Cleveland State University | Residual stress measurements in metal objects using four coils |
| CN103439206A (en) * | 2013-09-13 | 2013-12-11 | 徐州工程学院 | Micro-indentation-based method for testing residual stress of tiny area of tough block material |
| CN103604535A (en) * | 2013-11-27 | 2014-02-26 | 东南大学 | Residual stress testing structure based on difference capacitor bridge |
| CN103913789A (en) * | 2014-04-03 | 2014-07-09 | 大连理工大学 | Method for preparing high aspect ratio metal microgratings on metal substrate |
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2016
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5898302A (en) * | 1997-11-25 | 1999-04-27 | Cleveland State University | Residual stress measurements in metal objects using four coils |
| CN103439206A (en) * | 2013-09-13 | 2013-12-11 | 徐州工程学院 | Micro-indentation-based method for testing residual stress of tiny area of tough block material |
| CN103604535A (en) * | 2013-11-27 | 2014-02-26 | 东南大学 | Residual stress testing structure based on difference capacitor bridge |
| CN103913789A (en) * | 2014-04-03 | 2014-07-09 | 大连理工大学 | Method for preparing high aspect ratio metal microgratings on metal substrate |
Non-Patent Citations (1)
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| 微拉曼光谱技术及其在微结构残余应力检测中的应用;邱宇等;《机械强度》;20040830;第389-392页 |
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