CN105344694B - One kind removes carbide surface Al2O3With the method for TiCN composite coatings - Google Patents
One kind removes carbide surface Al2O3With the method for TiCN composite coatings Download PDFInfo
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- CN105344694B CN105344694B CN201510634839.5A CN201510634839A CN105344694B CN 105344694 B CN105344694 B CN 105344694B CN 201510634839 A CN201510634839 A CN 201510634839A CN 105344694 B CN105344694 B CN 105344694B
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- 238000000576 coating method Methods 0.000 title claims abstract description 62
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 48
- 239000000956 alloy Substances 0.000 claims abstract description 31
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 30
- 238000000498 ball milling Methods 0.000 claims abstract description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 23
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000012535 impurity Substances 0.000 claims abstract description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 11
- 238000010791 quenching Methods 0.000 claims abstract description 8
- 230000000171 quenching effect Effects 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000001238 wet grinding Methods 0.000 claims description 8
- 238000005336 cracking Methods 0.000 claims description 5
- 208000037656 Respiratory Sounds Diseases 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims 1
- 239000010931 gold Substances 0.000 claims 1
- 229910052737 gold Inorganic materials 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 12
- 239000000203 mixture Substances 0.000 abstract description 6
- 239000011247 coating layer Substances 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 238000009472 formulation Methods 0.000 abstract 1
- 230000035515 penetration Effects 0.000 abstract 1
- 239000000758 substrate Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 206010019233 Headaches Diseases 0.000 description 1
- 229910009043 WC-Co Inorganic materials 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Food Science & Technology (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Powder Metallurgy (AREA)
Abstract
One kind removes carbide surface Al2O3With the method for TiCN composite coatings, belong to Hardmetal materials and powder metallurgical technology.Using the thermal expansion coefficient difference of coating material and matrix material as point of penetration, the size and coating layer thickness of material are considered, comprehensive matrix material and the thermal conductivity of coating material and the difference of the coefficient of expansion, formulation carry Al2O3With quenching technical in the heating technique and liquid nitrogen of the hard alloy of TiCN composite coatings；To the sample after ball milling, heat treatment temperature and soaking time are determined according to matrix Co contents, the clean hard alloy block material of Composite coating removal is obtained after further ball milling.The present invention using equipment it is simple, do not introduce impurity, energy-conserving and environment-protective, and industrial-scale production can be realized, can thoroughly remove Al2O3Pure carbide matrix material is obtained with TiCN composite coatings.
Description
Technical field
The present invention relates to one kind to remove carbide surface Al2O3With the method for TiCN composite coatings, belong to hard alloy material
Material and powder metallurgical technology.
Background technology
Cutting element is one of important directions of Hardmetal materials application.Al2O3Have with TiCN composite coatings and apply thickness
Spend small (generally only ten a few to tens of microns), be firmly combined with hard alloy substrate, can increase substantially the wear-resisting of cutter and
Resistance to oxidation corrosive nature.Therefore, the hard alloy cutter with composite coating turns into the main product of cutting element application.With
Increasing for cutter application and quantity, has large quantities of cutters to scrap, these cutters scrapped contain substantial amounts of strategy every year
Elemental tungsten and rare metal cobalt, its recycling are paid attention to by various countries' relevant enterprise.These band coating cutters were reclaiming
Cheng Zhong, coating material turn into the impurity element in secondary alloy, have a strong impact on the performance and use range of alloy.Therefore, coating
The removal of carbide tool surface coating turns into the key technology of such Hardmetal materials regeneration.
Existing researcher is studied for the minimizing technology of carbide surface coating, such as chemistry point in chemical method
Solution, electrolysis, electrochemical process etc., these methods use substantial amounts of acid-base solution, very unfavorable to environment；Physical method such as from
Beamlet, sandblasting etc., have that cost is high, be easily introduced impurity, coating is difficult to remove the problems such as clean.Al2O3Layer resistance to oxidation and acid and alkali-resistance
Corrosion, TiCN layer and hard alloy substrate associativity are strong, and have inoxidizability.Therefore, the removal of the composite coating is current
Focus of attention and difficulties anxious to be resolved during hard alloy reclaiming.Therefore, hard carbide industry field is anxious
A kind of convenient, environment-friendly, practicality and high efficiency the carbide surface coating removal method of technique yet-to-be developed.
Present inventor develops one kind and is directed to carbide matrix body surface on the basis of many experiments exploratory development
Face Al2O3With the minimizing technology of TiCN composite coatings, Al is removed using this technology2O3With TiCN composite coatings, without using to environment
The acid-base solution polluted, minimizing technology is easy and effective, and can complete the reclaiming of hard alloy in batches.
The content of the invention
The present invention is for problem present in existing carbide surface coating removal, there is provided a kind of carbide surface
The minimizing technology of composite coating.Regardless of hard alloy composition, Al2O3Gross thickness with TiCN composite coatings is all at 5-30 μm
In the range of, can be clean by coating removal using this method.
The present invention is directed to the international headache of carbide surface coating removal, there is provided a kind of Al2O3With TiCN composite coatings
Minimizing technology.
To achieve the above object, technical scheme comprises the following steps：
(1) Al will be coated2O3With the hard alloy of TiCN composite coatings, heated under atmospheric environment, heating rate be 3~
10 DEG C/min, temperature rises to 700~1000 DEG C, held for some time；Sample after heating is immediately placed in liquid nitrogen and quenched, is obtained
To the sample of coating cracking；
(2) sample that step (1) obtains is placed in ball mill and carries out wet-milling, impurity is filtered off after ball milling, carry out drying and
Abrading-ball is removed, part coating shedding is obtained and coating carries the sample of crackle；Design parameter is preferred：Ball-milling medium is water, ratio of grinding media to material
For 0.5:1, abrading-ball is 1~6mm of diameter phi sintered carbide ball, and rotational speed of ball-mill is 80~150 revs/min, Ball-milling Time 20
~60 minutes；
(3) sample for obtaining step (2) is incubated 6~60 minutes, will heated under conditions of air, 700~1000 DEG C
Sample afterwards, which is placed directly within ball mill, carries out wet-milling, and impurity is filtered off after ball milling, dries and removes abrading-ball, finally obtains Al2O3With
The clean hard alloy block of TiCN Composite coating removals.Design parameter is preferred：Ball-milling medium is water, ratio of grinding media to material 0.5:1, mill
Ball is 3~8mm of diameter phi sintered carbide ball, and rotational speed of ball-mill is 80~150 revs/min, and Ball-milling Time is 10~30 minutes；
In step (1), the expansion and contraction of soaking time and cool time to coating and hard alloy substrate have important
Influence, crackle size to carbide surface coating and its conclusive effect is distributed with.The heating and thermal insulation time ensures matrix
Temperature it is uniform, enough expansion occurs for hard alloy substrate.Heat time t1=(10~30) V1/3Minute, wherein, V is base
The volume of body hard alloy, this volume are unit mm3Corresponding numerical value, preferably V=2.0~1000mm3.Quenching should in liquid nitrogen
Ensure the decline of substrate temperature, ensure that coating material temperature is rapidly reduced to liquid nitrogen temperature again, generation is drastically shunk, further
Increase the quantity and size of coating crack.Cool time t in liquid nitrogen2=(2~3) the d seconds, wherein, d is the thickness of coating, this
Thickness is numerical value, d=3~50 μm corresponding to unit μm.
It is preferred that when the matrix of the present invention is WC-Co hard alloy, the soaking time of step (3) is (2~3) CCoMinute, its
Middle CCoFor the content (mass percent) of Co in matrix hard alloy, parameter CCoSpan be：CCo=3~20.
Compared with the methods of existing chemical method for removing carbide surface coating, physical method, the present invention has such as
Lower advantage：
(1) present invention heats band coating Hardmetal materials in atmosphere, is quenched in liquid nitrogen, based on hard alloy
The difference of the thermal coefficient of expansion of matrix and coating material, makes specimen surface coating cracking, and crack distribution is uniform；Pass through ball milling
Mode will part cracking coating removal, in further heating process air entrance passage is provided, make in heating process
Matrix contacts with oxygen, aoxidizes, and generates the oxide of volumetric expansion, makes coating cracking and crushes；Utilize the crisp of oxide
Property, remaining coating and small amounts thing are removed by ball milling, obtains the clean hard alloy substrate of coating removal.It can see
Go out, no matter sample heating or liquid nitrogen in quench, the thermal change of each position of face coat is basically identical, therefore, this hair
It is bright except simple profile sample, be also particularly suitable for the removal of complicated shape specimen surface coating, and coating removal is uniform, thorough
Bottom.
(2) auxiliary material that implementation process of the present invention uses is liquid nitrogen and water, it is not necessary to which the chemical reagent such as acid, alkali, is one
The environmentally safe coating removal method of kind, and impurity is not introduced, fundamentally ensure to remove Hardmetal materials after removing coating
Cleaning.
(3) present invention process step is simple, and it is few to influence the factor of coating removal effect, beneficial to improving production efficiency, product
Quality and the stability for preparing material property.
To sum up, the present invention relatively has the minimizing technology of hard alloy coating, have coating removal completely, especially technology sheet
Body hardware device invests outstanding advantage, the technical characteristics of the invention such as seldom, environment-friendly, energy-saving and emission-reduction and is adapted to industrially scalable
Production.
Brief description of the drawings
The electron scanning micrograph of raw material specimen cross section in Fig. 1 embodiments 1；
The X-ray diffracting spectrum of sample after removing coating is removed in Fig. 2 Examples 1 and 2；
The electron scanning micrograph of specimen surface after removing coating is removed in Fig. 3 embodiments 1；
Heated in Fig. 4 embodiments 2 and liquid nitrogen of quenching after specimen surface electron scanning micrograph and chemical composition；
The electron scanning micrograph of specimen surface after removing coating is removed in Fig. 5 embodiments 2.
Embodiment
With reference in fact the present invention will be further described, but the present invention is not limited to following examples.
Embodiment 1：The sectional view of raw material is as shown in Figure 1.Matrix is WC-10Co hard alloy, is directly contacted with matrix
Coating composition is TiCN, and thickness is 9 μm, Al2O3The thickness of coating is 4 μm, is the superficial layer of sample, is directly contacted with the external world, former
The volume for expecting sample is 730mm3；Raw material is placed in Muffle furnace, is increased to 950 DEG C using 5 DEG C/min firing rate, insulation
240 minutes；Sample after heating is placed in liquid nitrogen and quenches 30s；Sample after quenching, which is placed in ball mill, carries out wet-milling, and it is joined
Number is：Ball-milling medium is water, ratio of grinding media to material 0.5:1, abrading-ball be diameter phi 3mm sintered carbide ball, rotational speed of ball-mill be 120 turns/
Minute, Ball-milling Time is 30 minutes；Impurity is filtered off after ball milling, is dried and gone abrading-ball；The sample of acquisition is placed in 850 DEG C
Carry out wet-milling after being heat-treated 20 minutes in Muffle furnace, ball-milling medium is water, ratio of grinding media to material 0.5:1, abrading-ball is the hard of diameter phi 3mm
Matter alloying pellet, rotational speed of ball-mill are 90 revs/min, and Ball-milling Time is 15 minutes；Impurity is filtered off after ball milling, dries and removes abrading-ball.Most
Shown in the X-ray diffracting spectrum such as Fig. 2 (a) for the hard alloy block being prepared eventually, its surface topography is as shown in Figure 3.Can be with
Find out, the hard alloy block thing of preparation is mutually pure, only WC and Co phase compositions.
Embodiment 2：The matrix of raw material is the WC-16Co hard alloy containing inhibitor, and TiCN coating layer thicknesses are 12 μm,
Al2O3Coating layer thickness is 6 μm, and alloy volume is 20mm3.Raw material is placed in Muffle furnace, using 8 DEG C/min firing rate liter
Height is incubated 50 minutes to 800 DEG C；Sample after heating is placed in liquid nitrogen and quenches 50s, specimen surface pattern and composition after quenching
As shown in Figure 4；Sample, which is placed in ball mill, after quenching carries out wet-milling, and its parameter is：Ball-milling medium is water, ratio of grinding media to material 0.5:1,
Abrading-ball is diameter phi 5mm sintered carbide ball, and rotational speed of ball-mill is 100 revs/min, and Ball-milling Time is 45 minutes；Filtered off after ball milling
Impurity, dried and gone abrading-ball；The sample of acquisition is placed in 1000 DEG C of Muffle furnace after being heat-treated 40 minutes and carries out wet-milling,
Ball-milling medium is water, ratio of grinding media to material 0.5:1, abrading-ball is diameter phi 8mm sintered carbide ball, and rotational speed of ball-mill is 110 revs/min,
Ball-milling Time is 10 minutes；Impurity is filtered off after ball milling, dries and removes abrading-ball.The X- for the hard alloy block being finally prepared is penetrated
For ray diffraction diagram spectrum as shown in Fig. 2 (b), its surface topography is as shown in Figure 5.As can be seen that the hard alloy block thing prepared is mutually pure
Only, only WC and Co phase compositions.
Claims (2)
1. one kind removes carbide surface Al2O3With the method for TiCN composite coatings, it is characterised in that comprise the following steps：
(1) Al will be coated2O3With the hard alloy of TiCN composite coatings, heated under atmospheric environment, heating rate be 3~10 DEG C/
Min, temperature rise to 700~1000 DEG C, held for some time；Sample after heating is immediately placed in liquid nitrogen and quenched, is applied
The sample of layer cracking；
(2) sample that step (1) obtains is placed in ball mill and carries out wet-milling, impurity is filtered off after ball milling, dried and gone to grind
Ball, obtains part coating shedding and coating carries the sample of crackle；
(3) sample for obtaining step (2) is incubated 6~60 minutes, after heating under conditions of air, 700~1000 DEG C
Sample, which is placed directly within ball mill, carries out wet-milling, and impurity is filtered off after ball milling, dries and removes abrading-ball, finally obtains Al2O3Answered with TiCN
Close the clean hard alloy block of coating removal；
Step (2) ball milling design parameter：Ball-milling medium is water, ratio of grinding media to material 0.5:1, the hard that abrading-ball is 1~6mm of diameter phi closes
Gold goal, rotational speed of ball-mill are 80~150 revs/min, and Ball-milling Time is 20~60 minutes；Step (1) heat time t1=(10~
30)V1/3Minute, wherein, V is the volume of matrix hard alloy, and this volume is unit mm3Corresponding numerical value, V=2.0~
8000mm3；Cooling Quenching time t in step (1) liquid nitrogen2=(2~3) the d seconds, wherein, d is the thickness of coating, and this thickness is single
Numerical value corresponding to position μm, d=3~50 μm.
2. according to the method for claim 1, it is characterised in that step (3) ball milling design parameter：Ball-milling medium is water, ratio of grinding media to material
For 0.5:1, abrading-ball is 3~8mm of diameter phi sintered carbide ball, and rotational speed of ball-mill is 80~150 revs/min, Ball-milling Time 10
~30 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510634839.5A CN105344694B (en) | 2015-09-29 | 2015-09-29 | One kind removes carbide surface Al2O3With the method for TiCN composite coatings |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510634839.5A CN105344694B (en) | 2015-09-29 | 2015-09-29 | One kind removes carbide surface Al2O3With the method for TiCN composite coatings |
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| Publication Number | Publication Date |
|---|---|
| CN105344694A CN105344694A (en) | 2016-02-24 |
| CN105344694B true CN105344694B (en) | 2017-12-29 |
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| CN201510634839.5A Active CN105344694B (en) | 2015-09-29 | 2015-09-29 | One kind removes carbide surface Al2O3With the method for TiCN composite coatings |
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Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60243285A (en) * | 1984-05-17 | 1985-12-03 | Permelec Electrode Ltd | Method for removing cover from metallic electrode |
| JPS6475687A (en) * | 1987-09-18 | 1989-03-22 | Tanaka Precious Metal Ind | Method for removing coating metal from metal oxide base material |
| CN1064716C (en) * | 1998-05-19 | 2001-04-18 | 自贡硬质合金厂 | Recovering and regenerating treating process for waste hard alloy |
| CN1696350A (en) * | 2005-06-17 | 2005-11-16 | 自贡科瑞德新材料有限责任公司 | Method for removing coat layer on surface of coated hard alloy |
| US7934393B2 (en) * | 2007-06-05 | 2011-05-03 | Johns Nanville | Process for recycling glass fiber |
| CN101525700A (en) * | 2009-04-28 | 2009-09-09 | 株洲硬质合金集团有限公司 | Recovery processing method of hard alloy scraps |
| CN102294488A (en) * | 2011-08-23 | 2011-12-28 | 浙江锐利硬质合金有限公司 | Tungsten cobalt hard alloy recycling process |
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