CN1129678C - Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film - Google Patents
Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film Download PDFInfo
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- CN1129678C CN1129678C CN 00108513 CN00108513A CN1129678C CN 1129678 C CN1129678 C CN 1129678C CN 00108513 CN00108513 CN 00108513 CN 00108513 A CN00108513 A CN 00108513A CN 1129678 C CN1129678 C CN 1129678C
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- Prior art keywords
- arc
- niobium
- titanium
- film
- continuously
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Links
- 238000000151 deposition Methods 0.000 title claims abstract description 10
- 238000007733 ion plating Methods 0.000 title claims abstract description 10
- 230000008021 deposition Effects 0.000 title claims abstract description 8
- RJSRQTFBFAJJIL-UHFFFAOYSA-N niobium titanium Chemical compound [Ti].[Nb] RJSRQTFBFAJJIL-UHFFFAOYSA-N 0.000 title claims description 13
- 238000010891 electric arc Methods 0.000 title claims description 5
- 238000005516 engineering process Methods 0.000 title description 3
- 239000010955 niobium Substances 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 16
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims abstract description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- CFJRGWXELQQLSA-UHFFFAOYSA-N azanylidyneniobium Chemical compound [Nb]#N CFJRGWXELQQLSA-UHFFFAOYSA-N 0.000 abstract 2
- 239000007769 metal material Substances 0.000 abstract 1
- 238000007747 plating Methods 0.000 abstract 1
- 239000010408 film Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012528 membrane Substances 0.000 description 3
- QFUKUPZJJSMEGE-UHFFFAOYSA-N 5-(hydroxymethyl)-1-(3-methylbutyl)pyrrole-2-carbaldehyde Chemical compound CC(C)CCN1C(CO)=CC=C1C=O QFUKUPZJJSMEGE-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910000997 High-speed steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005566 electron beam evaporation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000010884 ion-beam technique Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
The present invention belongs to the technical field of metallic material surface modification. The present invention comprises: the components when the film is deposited and grows to different thickness is controlled by regulating the continuous change with the time function of arc current of a metal cathode target for the arc ion plating of pure titanium and pure niobium in the plating process so as to a superhard titanium nitride and niobium nitride gradient film in which the cohesion is good and the hardness exceeds the peak hardness of a common titanium nitride and niobium nitride film. The method of the present invention has high deposition rate, wide component control range and easy operation.
Description
Technical field the invention belongs to the metal surface properties modification technical field.
The background technology titanium nitride membrane is plated on cutter or the die surface life-span is significantly improved, and has once caused cutting-tool engineering revolution widely in the eighties, and the rapid industrialization for the mechanical industry automatic production line provides key condition.In recent years, machine add industry will to more at a high speed and the serialization producer to developing and tool and mould will use under the rugged environment more, the simple HV2400 performance that titanium nitride membrane had can not satisfy this requirement fully.
Add other alloying elements and can improve and improve the performance of titanium nitride membrane, promptly embody polynary complex intensifying effect; Gradient material be meant key element such as the component, structure, concentration of constituent material along on the thickness direction by a side direction opposite side slowly transition continuously, thereby make material possess certain more excellent performance.For the gradient hard thin-film material, because methods such as domestic main employing magnetron sputtering, hollow cathode, electron beam evaporation ion plating and ion beam assisted depositing are synthesized at present, because of its workpiece Heating temperature height, sedimentation rate is low, the composition regulation range is little, often makes the film that has designed gradient composition and structure be difficult to realize on technology.
Summary of the invention the purpose of this invention is to provide that a kind of relative depositing temperature is low, speed is fast, the composition regulation range is wide, the method with the superhard matter gradient film of electric arc ion-plating deposition titanium niobium nitride of a kind of novel titanium nitride base composite ganoine gradient film of preparation easy and simple to handle.
Technical solution of the present invention is; workpiece is put into the equipment vacuum chamber through behind the cleaning-drying; through vacuumizing; logical argon gas; open arc; add negative bias; sputter clean; logical nitrogen; plated film; stop arc; outage; stove takes out workpiece after the cold stage such as grade; its special; in the plated film stage; select pure titanium and pure niobium to make cathode targets; two kinds of targets place on the arc source position of arc ion plating separately; when plated film began, it is constant that the titanium arc stream is transferred to 62～68A, opens the niobium arc; in 35～45 minutes; the niobium arc stream evenly is adjusted to 88～95A, in this course titanium niobium nitride (Ti continuously from 100～105A
XNb
1-X) x among the N increases from 0.33～0.36 with film thickness and rise to 0.39～0.41 continuously, next the niobium arc stream remained unchanged, and in 18～22 minutes, again the titanium arc stream evenly is adjusted to 73～78A, titanium niobium nitride (Ti continuously
XNb
1-X) x among the N further rises to 0.43～0.46 with the growth of film thickness continuously from 0.39～0.41.Composition when the film dynamic growth is controlled in the continuous variation of the arc current time function by regulating two kinds of targets to different thickness, the synthetic superhard matter gradient film of titanium niobium nitride of deposition makes that synthetic film internal stress is little, the inboard is combined, outside hardness height.
Effect of the present invention is to synthesize with film thickness to increase by lining and table titanium niobium nitride (Ti
XNb
1-X) x among the N varies continuously to 0.43～0.46 titanium niobium nitride gradient film from 0.33～0.36, having slowed down internal stress is combined film and workpiece, simultaneously have superhard characteristic again, on high speed steel substrate, surpass its common titanium niobium nitride film maximum hardness HV3400, and reach HV3800.
The present invention is described further below in conjunction with embodiment for embodiment.
The rapid steel workpiece is put into the equipment vacuum chamber through behind the cleaning-drying, and pure titanium and pure niobium target place on the arc source position of arc ion plating separately, are evacuated down to 10
-2Pa, logical argon gas opens the titanium arc to 0.5Pa, arc stream fixes on 60A, add negative bias to be pressed onto-1000V carried out sputter clean 5 minutes, stopped argon gas, logical nitrogen to 0.4Pa, and negative bias drops to-300V, the beginning plated film, it is constant that the titanium arc stream is transferred to 65A, opens the niobium arc, in 40 minutes, the niobium arc stream evenly is adjusted to 90A, (Ti in this course continuously from 102A
XNb
1-X) x among the N increases from 0.35 with film thickness and rise to 0.40 continuously, and the niobium arc stream is remained unchanged, and in 20 minutes, again the titanium arc stream evenly is adjusted to 75A, (Ti continuously
XNb
1-X) x among the N further rises to 0.45 with the growth of film thickness continuously from 0.40, stop arc after then, stop the supple of gas or steam, outage, stove bleeds off vacuum and takes out the rapid steel workpiece after cold 1 hour.The superhard matter gradient film of deposition synthetic titanium niobium nitride, from inside to outside hardness changes from low to high continuously, and inboard good with the workpiece film-substrate cohesion, outside hardness height has superhard characteristic, surpasses the maximum hardness HV3400 of common titanium niobium nitride film, reaches HV3800.
Claims (2)
1. use the method for the superhard matter gradient film of electric arc ion-plating deposition titanium niobium nitride; workpiece is put into the equipment vacuum chamber through behind the cleaning-drying; through vacuumizing; logical argon gas; open arc; add negative bias; sputter clean; logical nitrogen; plated film; stop arc; outage; stove is cold; take out workpiece after stage; it is characterized in that: in the plated film stage; select pure titanium and pure niobium to make cathode targets; two kinds of targets place on the arc source position of arc ion plating separately; when plated film begins; it is constant that the titanium arc stream is transferred to 62～68A; open the niobium arc, in 35～45 minutes, the niobium arc stream is from 100～105A; evenly be adjusted to 88～95A continuously; next the niobium arc stream is remained unchanged, in 18～22 minutes, again the titanium arc stream evenly is adjusted to 73～78A continuously.
2. the method with the superhard matter gradient film of electric arc ion-plating deposition titanium niobium nitride according to claim 1, it is characterized in that: in the plated film stage, it is constant during beginning the titanium arc stream to be transferred to 65A, open the niobium arc, in 40 minutes, the niobium arc stream evenly is adjusted to 90A continuously from 102A, next the niobium arc stream is remained unchanged, in 20 minutes, again the titanium arc stream evenly is adjusted to 75A continuously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00108513 CN1129678C (en) | 2000-04-28 | 2000-04-28 | Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00108513 CN1129678C (en) | 2000-04-28 | 2000-04-28 | Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1321790A CN1321790A (en) | 2001-11-14 |
| CN1129678C true CN1129678C (en) | 2003-12-03 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 00108513 Expired - Fee Related CN1129678C (en) | 2000-04-28 | 2000-04-28 | Electric arc ion-plating deposition technology of titanium niobium nitride superhard gradient film |
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| Country | Link |
|---|---|
| CN (1) | CN1129678C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1306060C (en) * | 2002-06-21 | 2007-03-21 | 王殿儒 | Method for treating tin soldering wettability by using cathode electric arc ion plating technology |
| CN1316058C (en) * | 2005-03-24 | 2007-05-16 | 上海交通大学 | Method for modifying surface of polymer microffow chip by sputtering TiO2 |
| CN101705471B (en) * | 2009-11-30 | 2011-06-15 | 沈阳大学 | Preparation method of chromium nitride titanium aluminum nitrogen gradient hard reaction film |
| CN101709450B (en) * | 2009-11-30 | 2011-06-15 | 沈阳大学 | Method for preparing zirconium-titanium-aluminum-nitrogen nitride gradient hard reaction film |
| CN114411098A (en) * | 2021-12-21 | 2022-04-29 | 嘉兴岱源真空科技有限公司 | Coating method of TiNb coating |
| CN114561622B (en) * | 2022-01-14 | 2024-04-26 | 西安理工大学 | Gradient structure Ti-Nb alloy film and preparation method thereof |
-
2000
- 2000-04-28 CN CN 00108513 patent/CN1129678C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1321790A (en) | 2001-11-14 |
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