CN103926132A - Hard alloy cutter surface coating etchant and application method thereof - Google Patents

Hard alloy cutter surface coating etchant and application method thereof Download PDF

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Publication number
CN103926132A
CN103926132A CN201410180602.XA CN201410180602A CN103926132A CN 103926132 A CN103926132 A CN 103926132A CN 201410180602 A CN201410180602 A CN 201410180602A CN 103926132 A CN103926132 A CN 103926132A
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sample
coating
etchant
polishing
ultrasonic cleaning
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CN201410180602.XA
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王周成
张倍源
吴正涛
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Xiamen University
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Xiamen University
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Abstract

The invention discloses a hard alloy cutter surface coating etchant and an application method of the hard alloy cutter surface coating etchant, and relates to an alloy cutter. The etchant consists of HNO3, HCl, HF and H2O according to a volume ratio of 35: (0-10): 10: (5-15) of the HNO3 to the HCl to the HF to the H2O. The application method comprises the following steps: preparing a hard alloy coated cutter sample into a cylindrical sample, taking phenolic resin powder as an enchasing filler, molding the sample and taking out, sequentially grinding, washing with ultrasonic wave, drying, polishing and washing with ultrasonic wave again; washing the sample with ultrasonic wave by use of deionized water, subsequently washing with absolute ethyl alcohol, drying, putting the sample into the hard alloy cutter surface coating etchant for etching, taking out after etching, swashing with water, then putting the sample into the absolute ethyl alcohol to wash with ultrasonic wave again, baking, drying, and observing through a scanning electron microscope to obtain a coated microscopic structure. The hard alloy cutter surface coating etchant can be used for effectively displaying an HT-CVD (Chemical Vapor Deposition) aluminum oxide coated microscopic structure on the surface of a hard alloy cutter so as to achieve the aims of displaying the size and structure of coating grains and distinguishing grain boundaries of the coating grains.

Description

A kind of carbide tool surface coating etchant and using method thereof
Technical field
The present invention relates to alloy cutter, especially relate to a kind of carbide tool surface coating etchant and using method thereof.
Background technology
Along with popularizing of numerically-controlled machine and machining center, efficient high-speed high precision has cut into the main development direction of modern processing, to the performance of cutter is corresponding, also has higher requirement.It is to improve one of important channel of cutting performance that cutter carries out coating processing.Cutting-Tool Coating Technology had been obtained major progress in recent years.Cutting tool surface coatingization mainly realizes by physical vapour deposition (PVD) and two kinds of depositing operations of chemical vapor deposition, wherein chemical vapor deposited coatings remains the main coating process of indexable insert tip, throw away tip, MT-CVD (middle temperature chemical vapor deposition) titanium carbonitride, HT-CVD (high temperature chemical vapor deposition have been developed, high temperature chemical vapor deposition) new technology (S.Ruppi, A.Larsson.THIN SOLID FILMS388 (2001) 50-61 such as thick film aluminium oxide, P.Hanssona, M.Halvarssona, S.Vuorinenb.SURFACE AND COATINGS TECHNOLOGY76-77 (1995) 256-264), new coating, wherein aluminum oxide coating layer has the mechanics of many excellences, physical property, as high in hardness, wear-resisting, high-temperature stability and chemical stability are good, so aluminum oxide coating layer is as wear-resistant coating, be applied to carbide cutting blade, the mechanical part of at high temperature working and the various fields (M.Halvarssona such as anticorrosive, and S.Vuorinenb.SURFACE AND COATINGS TECHNOLOGY80 (1996) 80-88, M.Halvarssona and S.Vuorinenb.MATERIALS SCIENCE AND ENGINEERING A209 (1996) 337-344).Fine grain aluminum oxide coating layer at titanium carbonitride coating surface deposition not only has very high abrasion resistance properties, and can effectively make up the defect (M.Halvarssona, J.E.Trancika and S.Ruppib.INTERNATIONAL JOURNAL OF REFRACTORY METALS & HARD MATERIALS24 (2006) 32-38) that nexine titanium carbonitride material is anti-oxidant under hot conditions, ability is worn and torn in antisticking.
The microstructure of carbide tool surface coating is one of deciding factor of the mechanical property qualities such as the bond strength of coating microhardness, coating and matrix and coating high-temp rubbing wear, therefore the necessary means of evaluating product quality is not only in the microstructural analysis of coating, more contributes to improve preparation technology of coating.Because hard alloy coating has hard, crisp, thinly, general section sample preparation is more difficult, simultaneously less about the etchant research of the thin brilliant single-phase coating of hard both at home and abroad, institutional framework data deficiencies.
The sample preparation of thin brilliant single-phase coating microstructure analysis, comprising: inlay, grinding, polishing, four steps of etch.Inlay general employing hot pressing inlaying process, take phenolics powder as inserts, on hot pressing mounting press, carry out; Grinding is the committed step in metallographic specimen preparation process, and sample, after polishing, has trickle polishing scratch and surface to still have the deformation disturbance layer of metal, affects correct display organization, therefore necessary polishing; Polished sample, requires to reach flour milling as bright as a sixpence, the effect of complete each phase of reservation.Polished specimen surface is as bright as a sixpence, but can only see snotter, pore and crack etc. while examining under a microscope, and the microstructure that analyze, observe sample is even distinguished the crystal boundary of surface coating, the operation that sample also must show through tissue.The method that tissue shows mainly can be divided into two large classes: chemical method and Physical.The former generally includes chemical reagent etch, electro-etching, oxidizing process etc.; The latter comprises heat etching, vacuum coating, cathode ion etching, method of magnetic etc.We adopt chemical reagent etch method to process the microstructure analysis that polished sample carries out thin brilliant single-phase coating.Sample is under certain density chemical reagent effect, can not only dissolve surperficial upset layer, main is can make between the various tissues of alloy, intercrystalline or the grain boundaries of monophase materials are subject to erosion in various degree because corrosion resistance is different, the rugged structure in surface presenting after this being etched can present light and shade contrast while examining under a microscope, thereby reach, shows microstructural object.
Coating displaing microstructure observing can adopt metaloscope, scanning and transmission electron microscope, and the coated grains of preparing due to vapour deposition is of a size of submicron order, so the low optical microscope of resolution cannot be for the microstructural analysis of coating; Although current transmission electron microscope coupled ion reduction can obtain some information, make sample very complicated, can not follow the tracks of in good time.It is high that scanning electron microscope has resolution, and the depth of field is large, can be used as convenient, fast, effective, the reliable characterization method of coating microstructure analysis.
Summary of the invention
Object of the present invention aims to provide and can effectively show carbide tool surface HT-CVD aluminum oxide coating layer microstructure, to reach a kind of carbide tool surface coating etchant and the using method thereof that shows crystal boundary object between the size of coated grains and structure, differentiation coated grains.
Described carbide tool surface coating etchant consisting of by volume: HNO 3: HCl: HF: H 2o=35: (0~10): 10: (5~15).
Described HNO 3the massfraction massfraction that can be 65%~68%, HCl can be 36%~38%, HF massfraction can>=40%.
The using method of described carbide tool surface coating etchant is as follows:
1) carbide alloy coating cutter sample is made to cylinder sample, with phenolics powder, for inlaying filler, after sample moulding, take out, grind successively, ultrasonic cleaning, dries polishing, again ultrasonic cleaning;
2) sample is used to deionized water ultrasonic cleaning, with absolute ethyl alcohol, clean again, after oven dry, sample is put into the etch of carbide tool surface coating etchant, after etch, take out, water rinses, again sample is placed in to absolute ethyl alcohol ultrasonic cleaning again, dries, dry, electron microscopic observation to be scanned, obtains being coated with layer microstructure.
In step 1) in, describedly carbide alloy coating cutter sample is made to cylinder sample carbide alloy coating cutter sample can be made on hot pressing pointing machine to the regular cylinder sample of diameter 30mm; The described consumption of inlaying filler can be 12~15g; The temperature of described moulding can be 130 ℃; The method of described grinding can be roughly ground the sample of having inlayed and fine grinding respectively on 600 orders and 1200 object boart boart wheel discs, and the time of corase grind and fine grinding all can be 3~8min, and described grinding can adopt automatic grinding and polishing device, and rotating speed is 500r/min; The time of described ultrasonic cleaning can be 2min; The method of described polishing can be carried out polishing with the diamond polishing powder of W2.5 by sample, and the time of polishing can be 10min; Described ultrasonic cleaning again can be placed on the sample after polishing ultrasonic cleaning 5min in absolute ethyl alcohol, to remove the impurity such as the greasy dirt of specimen surface in polishing process and burnishing powder.
In step 2) in, the time of described ultrasonic cleaning can be 2min; The time of described etch can be 30~40s, and the temperature of etch can be 30 ℃; The time of described ultrasonic cleaning again can be 2min.
The present invention adopts that hot pressing is inlayed, grinding and polishing has been prepared the cross section sample of alumina coated cutting tool in conjunction with the metallography preparation method of ultrasonic cleaning, with chemical etching method, by scanning electron microscopic observation, obtains the microstructure of coating.In the process of chemical etching, selection test through etchant repeatedly: the etching solutions such as nitric acid+hydrofluorite, nitric acid+hydrochloric acid, nitric acid+hydrochloric acid+hydrofluorite, the concentrated sulphuric acid, nitric acid+acetic acid, consider its etch rate and etch effect, choose nitric acid, hydrofluorite and salt aqueous acid as etchant, can reach the column structure that shows aluminum oxide coating layer, obtain the size of crystal grain, effectively distinguish the crystal boundary between columnar grain.The present invention provides effective means for the characterization research of coating structure and performance.
Accompanying drawing explanation
Fig. 1 is the Cross Section Morphology SEM figure (* 10000) of coating after embodiment 1 etchant etch.
Fig. 2 is the Cross Section Morphology SEM figure (* 10000) of coating after embodiment 2 etchant etches.
Fig. 3 is the Cross Section Morphology SEM figure (* 10000) of coating after embodiment 3 etchant etches.
Fig. 4 is the Cross Section Morphology SEM figure (* 10000) of coating after embodiment 4 etchant etches.
Fig. 5 is HT-CVD aluminum oxide coating layer surface topography SEM figure (* 10000).
Embodiment
Embodiment 1
1. sample preparation: (1) hot pressing is inlayed: sample thief (the aluminium oxide hard coated cutting tool that high temperature chemical vapor deposition legal system is standby), the phenolics powder of take is made the regular cylinder sample of diameter 30mm as filler on hot pressing pointing machine, and forming temperature is 130 ℃, pressure heat-preserving 5min.(2) grind: the sample of having inlayed is roughly ground fully and fine grinding respectively on 600 orders and 1200 object boart boart wheel discs, the time of thickness mill is controlled at 5min left and right, more than grind and all adopt automatic grinding and polishing device, rotating speed is 500r/min, not open close chilled water in process of lapping, slightly, between fine lapping, to carry out sufficient ultrasonic cleaning (ultrasonic cleaning time 2min in absolute ethyl alcohol) and with 100 ℃ of oven for drying, to remove abrasive dust and greasy dirt to sample.
(3) polishing: sample is through after grinding, then carry out polishing with the diamond polishing powder of W2.5, polishing time is 10min, simultaneously the reasonable consumption of control chilled water in polishing process; After polishing completes, sample is placed in absolute ethyl alcohol, ultrasonic cleaning 5min, to remove the greasy dirt of specimen surface in polishing process and burnishing powder impurity etc.
2. the preparation of etchant: measure the dense HNO of 35ml with glass cylinder respectively 3with 15ml H 2o is added in plastic beaker, then with plastic cylinder, measures the dense HF of 10ml and be added in beaker, puts to ultrasonic 2min in ultrasonic device to solution and evenly mixes.
3. etch operation: before etch, first by deionized water ultrasonic cleaning 2min for sample, with absolute ethyl alcohol, clean again, after 100 ℃ of oven for drying, sample is put into etchant (30 ℃ of waters bath with thermostatic control), after etch 40s, take out, water rinses, then sample is placed in to absolute ethyl alcohol ultrasonic cleaning 2min, through oven for drying, be placed in exsiccator and preserve, electron microscopic observation to be scanned.
Fig. 1 is the Cross Section Morphology of sample after etch, can be observed the microstructure of the irregular prism-shaped of aluminum oxide coating layer by Fig. 1, and the direction of growth of coated crystal.
Embodiment 2
1. sample preparation: (1) hot pressing is inlayed: with embodiment 1.(2) grind: with embodiment 1.(3) polishing: with embodiment 1.
2. the preparation of etchant: measure the dense HNO of 35ml with glass cylinder respectively 3, the dense HCl of 5ml and 10ml H 2o is added in plastic beaker, then with plastic cylinder, measures the dense HF of 10ml and be added in beaker, puts to ultrasonic 2min in ultrasonic device to solution and evenly mixes.
3. etch operation: carry out etch with embodiment 1, the etch time is 30s.
Fig. 2 is the Cross Section Morphology of sample after etch, with embodiment 1, compares, and during etchant forms, the volume of concentrated hydrochloric acid increases, but the time of etch is reduced to 30s, comparative example's 1 pattern is found, shows that the region of prismatic structure increases in coating, also can observe the crystal boundary of part intergranule.
Embodiment 3
1. sample preparation: (1) hot pressing is inlayed: with embodiment 1.(2) grind: with embodiment 1.(3) polishing: with embodiment 1.
2. the preparation of etchant: measure the dense HNO of 35ml with glass cylinder respectively 3, the dense HCl of 5ml and 10ml H 2o is added in plastic beaker, then with plastic cylinder, measures the dense HF of 10ml and be added in beaker, puts to ultrasonic 2min in ultrasonic device to solution and evenly mixes.
3. etch operation: carry out etch with embodiment 1, time 40s.
Fig. 3 is the Cross Section Morphology of sample after etch, in this routine etchant, the volume of hydrochloric acid is compared with example 1 to some extent increases, than embodiment 2, the etch time increases to 40s, can clearly observe the irregular prism-shaped crystal grain of aluminum oxide coating layer and the crystal growth pattern of column, also can effectively distinguish the crystal boundary of intergranule from figure simultaneously.Therefore when the volume of concentrated hydrochloric acid and etch time are all increased to a certain degree, can reach the microstructural object of demonstration coating.
Embodiment 4
1. sample preparation: (1) hot pressing is inlayed: with embodiment 1.(2) grind: with embodiment 1.(3) polishing: with embodiment 1.
2. the preparation of etchant: measure the dense HNO of 35ml with glass cylinder respectively 3, the dense HCl of 10ml and and 5ml H 2o is added in plastic beaker, then with plastic cylinder, measures the dense HF of 10ml and be added in beaker, puts to ultrasonic 2min in ultrasonic device to solution and evenly mixes.
3. etch operation: carry out etch with embodiment 1, etch time 40s.
Fig. 4 is the Cross Section Morphology of sample after etch, from figure, observe and can find, along with concentrated hydrochloric acid volume increases, etch depth also has increase to a certain degree, coatings and substrate has coming off in various degree, so the concentrated hydrochloric acid volume in etchant and etch time should not surpass 10ml and 40s.

Claims (10)

1. a carbide tool surface coating etchant, is characterized in that consisting of by volume: HNO 3: HCl: HF: H 2o=35: (0~10): 10: (5~15).
2. a kind of carbide tool surface coating etchant as claimed in claim 1, is characterized in that described HNO 3the massfraction massfraction that is 65%~68%, HCl massfraction>=40% that is 36%~38%, HF.
3. the using method of carbide tool surface coating etchant as claimed in claim 1, is characterized in that its step is as follows:
1) carbide alloy coating cutter sample is made to cylinder sample, with phenolics powder, for inlaying filler, after sample moulding, take out, grind successively, ultrasonic cleaning, dries polishing, ultrasonic cleaning;
2) sample is used to deionized water ultrasonic cleaning, with absolute ethyl alcohol, clean again, after oven dry, sample is put into the etch of carbide tool surface coating etchant, after etch, take out, water rinses, again sample is placed in to absolute ethyl alcohol ultrasonic cleaning again, dries, dry, electron microscopic observation to be scanned, obtains being coated with layer microstructure.
4. the using method of carbide tool surface coating etchant as claimed in claim 3, it is characterized in that in step 1) in, it is described that carbide alloy coating cutter sample is made to cylinder sample is carbide alloy coating cutter sample to be made on hot pressing pointing machine to the regular cylinder sample of diameter 30mm.
5. the using method of carbide tool surface coating etchant as claimed in claim 3, is characterized in that in step 1) in, described in inlay filler consumption be 12~15g; The temperature of described moulding can be 130 ℃.
6. the using method of carbide tool surface coating etchant as claimed in claim 3, it is characterized in that in step 1) in, the method of described grinding is that the sample of having inlayed is roughly ground and fine grinding respectively on 600 orders and 1200 object boart boart wheel discs, the time of corase grind and fine grinding all can be 3~8min, described grinding can adopt automatic grinding and polishing device, and rotating speed is 500r/min.
7. the using method of carbide tool surface coating etchant as claimed in claim 3, is characterized in that in step 1) in, the time of described ultrasonic cleaning is 2min; Described ultrasonic cleaning again can be placed on the sample after polishing ultrasonic cleaning 5min in absolute ethyl alcohol.
8. the using method of carbide tool surface coating etchant as claimed in claim 3, is characterized in that in step 1) in, the method for described polishing is that sample is carried out to polishing with the diamond polishing powder of W2.5, the time of polishing is 10min.
9. the using method of carbide tool surface coating etchant as claimed in claim 3, is characterized in that in step 2) in, the time of described ultrasonic cleaning is 2min; The time of described ultrasonic cleaning again can be 2min.
10. the using method of carbide tool surface coating etchant as claimed in claim 3, is characterized in that in step 2) in, the time of described etch is 30~40s, the temperature of etch is 30 ℃.
CN201410180602.XA 2014-04-30 2014-04-30 Hard alloy cutter surface coating etchant and application method thereof Pending CN103926132A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105067414A (en) * 2015-08-17 2015-11-18 江西稀有稀土金属钨业集团有限公司 System and method for observing hard alloy structure with scanning electron microscope
CN106826408A (en) * 2017-02-09 2017-06-13 同济大学 A kind of lbo crystal polishing method based on crystal oxidant
CN109338366A (en) * 2018-11-23 2019-02-15 东南大学 A kind of titanium-based hard conating remanufactured towards cutter moves back coating method
CN110672398A (en) * 2019-10-14 2020-01-10 飞而康快速制造科技有限责任公司 Sample preparation method for titanium alloy metallographic sample

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101353794A (en) * 2008-09-03 2009-01-28 董加坤 Austenitic stainless steel metallographic etchant, preparing method and use thereof
CN101603894A (en) * 2009-07-16 2009-12-16 厦门大学 A kind of etching agent for titanium carbonitride coating on surface of hard alloy cutter and using method thereof
CN101603895A (en) * 2009-07-16 2009-12-16 厦门大学 A kind of etching agent for alumina coating on surface of hard alloy cutter and using method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101353794A (en) * 2008-09-03 2009-01-28 董加坤 Austenitic stainless steel metallographic etchant, preparing method and use thereof
CN101603894A (en) * 2009-07-16 2009-12-16 厦门大学 A kind of etching agent for titanium carbonitride coating on surface of hard alloy cutter and using method thereof
CN101603895A (en) * 2009-07-16 2009-12-16 厦门大学 A kind of etching agent for alumina coating on surface of hard alloy cutter and using method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105067414A (en) * 2015-08-17 2015-11-18 江西稀有稀土金属钨业集团有限公司 System and method for observing hard alloy structure with scanning electron microscope
CN106826408A (en) * 2017-02-09 2017-06-13 同济大学 A kind of lbo crystal polishing method based on crystal oxidant
CN109338366A (en) * 2018-11-23 2019-02-15 东南大学 A kind of titanium-based hard conating remanufactured towards cutter moves back coating method
CN109338366B (en) * 2018-11-23 2020-09-11 东南大学 Tool remanufacturing-oriented coating removing method for titanium-based hard coating
CN110672398A (en) * 2019-10-14 2020-01-10 飞而康快速制造科技有限责任公司 Sample preparation method for titanium alloy metallographic sample

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