CN106756783A - It is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film - Google Patents
It is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film Download PDFInfo
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- CN106756783A CN106756783A CN201611183942.3A CN201611183942A CN106756783A CN 106756783 A CN106756783 A CN 106756783A CN 201611183942 A CN201611183942 A CN 201611183942A CN 106756783 A CN106756783 A CN 106756783A
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- tantalum
- spinneret
- tantalum spinneret
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C8/00—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C8/06—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases
- C23C8/36—Solid state diffusion of only non-metal elements into metallic material surfaces; Chemical surface treatment of metallic material by reaction of the surface with a reactive gas, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using gases using ionised gases, e.g. ionitriding
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Spinning Methods And Devices For Manufacturing Artificial Fibers (AREA)
Abstract
The invention discloses a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film.Comprise the following steps：(1) surface of tantalum spinning jet is polished to more than 0.02 μm；(2) tantalum spinneret after surface is polished is cleaned and dried；(3) tantalum spinneret after cleaning is detected with microscope, is put into stove if without any pollution, it is 5 × 10 that vacuum will be evacuated in stove2Pa, temperature is raised to 500-700 DEG C, and hydrogen and nitrogen are added after 1-1.5h of insulation, wherein, the volume ratio of hydrogen and nitrogen is (4.5-5.5):1, with cooling water cooling, tantalum spinneret is taken out when in-furnace temperature is down to below 100 DEG C；(4) tantalum spinneret of taking-up is cleaned and is dried；(5) tantalum spinneret after cleaning is detected with microscope, is put into stove if without any pollution, DLC film is plated in surface of tantalum spinning jet with the method for magnetron sputtering；The target that plated film is used is acetylene, and plating conditions are as follows：Vacuum is 5 × 10‑3—8×10‑3Pa, 180-280 DEG C of temperature, sputtering time is 1-3h；Tantalum spinneret is cooled to less than 100 DEG C after plated film.
Description
Technical field
The present invention relates to a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film.
Background technology
Spinning head is the important spinning original basic part of textile of chemical fibre enterprise, and the quality of its quality directly influences synthetic fiber spinning
The mechanical performance of machine.The material for manufacturing spinning head mainly has the materials such as gold-platinum (Au-Pt), tantalum, it is desirable to which spinning head has high hard
Degree, high-wearing feature, surface roughness are high, have good spinnability.Because golden platinum spinning head is expensive, domestic enterprise's tantalum sprays
Silk head surface nitriding or the advance surface carburization of tantalum spinneret in anodized, but by the spinneret hole of anodized
Road roughness reduction, makes the spinnability of spinning head and using not as golden platinum spinning head.
The content of the invention
It is contemplated that overcoming the deficiencies in the prior art, there is provided a kind of in surface of tantalum spinning jet nitriding and to plate the side of DLC film
Method.
In order to achieve the above object, the technical scheme of present invention offer is：
It is described in surface of tantalum spinning jet nitriding and to plate the method for DLC film and comprise the following steps：
(1) surface of tantalum spinning jet is polished to more than 0.02 μm；
(2) tantalum spinneret after surface is polished is cleaned and dried；
(3) tantalum spinneret after cleaning is detected with microscope, be put into stove if without any pollution (will divide 7 layers in stove
Put, each interval 80mm, top layer must be covered), it is 5 × 10 that vacuum will be evacuated in stove2Pa, temperature is raised to 500-
700 DEG C, hydrogen and nitrogen are added after 1-1.5h of insulation, wherein, the volume ratio of hydrogen and nitrogen is (4.5-5.5):1, preferably 5：1, use
Cooling water cooling, tantalum spinneret is taken out when in-furnace temperature is down to below 100 DEG C；
(4) tantalum spinneret of taking-up is cleaned and is dried；
(5) tantalum spinneret after cleaning is detected with microscope, is put into stove (each tantalum spinneret if without any pollution
Distance is unanimously uniform), plate DLC film in surface of tantalum spinning jet with the method for magnetron sputtering；The target that plated film is used is acetylene,
Plating conditions are as follows：Vacuum is 5 × 10-3—8×10-3Pa, 180-280 DEG C of temperature, sputtering time is 1-3h；After plated film
Tantalum spinneret is cooled to less than 100 DEG C, the tantalum spinneret of plated surface DLC film is obtained final product.
Preferably, step (2) and the cleaning described in (4) is that the tantalum spinneret after first surface is polished is 98% in concentration
In sulfuric acid, carry out boiling 25-35min of acid treatment, preferably 30min under the conditions of 140 DEG C, spent again after then being rinsed with clear water
Ionized water is cleaned, then is cleaned by ultrasonic successively with alcohol, acetone and deionized water in ultrasonic cleaning tank.
Preferably, step (3) and (5) described microscope are the measuring microscope of 150 times of amplification.
Preferably, step (5) described sputtering time is 60-80min.
The invention will be further described below：
It is each 10 minutes that tantalum spinneret is boiled twice of sour 140 DEG C/30 minutes → clear water flushings → deionized water cleaning by the present invention,
Tantalum spinneret is put into stove, temperature is raised to 500-700 DEG C, be incubated 1 hour, it is 5 × 10 that vacuum is evacuated to vacuum2Pa,
(ratio is 5 to add High Purity Hydrogen (99.99%) and High Purity Nitrogen (99.99%):1), body of heater cooling water cooling, furnace body temperature is dropped to
Less than 100 DEG C, workpiece is taken out, surface forms TaN and amorphous layer.Again tantalum spinneret after ionic nitriding boil acid → rinse → go
Ionized water cleaning → alcohol → acetone → deionized water is respectively washed 10 minutes, tantalum spinneret is hung on the hook in stove, shuts stove
Door.The distance and position for hanging over hook is suitable, it is ensured that the inside and outside portion of tantalum spinneret is uniformly plated to, and coated stove preheating handle is vacuumized
It is 5 × 10 to vacuum-3—8×10-3Pa, temperature is raised to 180 DEG C -280 DEG C, and sputtering time is 1-3 hours, treats that temperature is dropped to
100 DEG C, workpiece is taken out.Material source of the invention is pressed into tantalum bar and is put into incipient fusion in 99.95% tantalum powder, through powder metallurgy process
After stove is through 2400-2600 DEG C of high temperature sintering, rolling is directly forged in flakes, HV80-100 or so is reached by hardness after annealing,
Elongation percentage more than 38%, by punch forming, be made after blank stamping parts bottom automatic numerical control puncher punching 2100 ×
0.055 hole, by making spinning head surface roughness reach more than 0.01um after grinding and polishing, then with 18 hertz of 300W frequencies
Supersonic cleaning machine is cleaned.
The present invention oozes last layer nitrogen, table beforehand through glow discharge nitriding in surface of tantalum spinning jet on the surface of tantalum spinneret
Face turns into interstitial solid solution, and case hardness is improved, and recycles the method plating last layer DLC film of magnetron sputtering, can so improve
The corrosion resistance of the case hardness, channel surfaces finish and spinning head of spinning head.
Compared with prior art, beneficial effects of the present invention are：
(1) after surface of tantalum spinning jet nitriding, surface forms interstitial solid solution and plates last layer DLC film again, can carry significantly
The case hardness of spinning head high, spinning head intensity and corrosion resistance, also improve duct finish, and relatively low coefficient of friction
Make the spinnability of spinning head more preferable.
(2) production efficiency of synthetic fiber spinning is improve, and price only has 1/4 or so of yellow platinum alloy.
Specific embodiment
Tantalum spinneret is the shape for hat spinning heads of Ф 16, and aperture is 0.055mm, and purity is 99.95%, and equipment is ionic nitriding
Stove.
Concretely comprise the following steps：Tantalum spinneret is boiled sour 140 DEG C/30 minutes → clear water flushing → deionized water to clean twice each 10
Minute, tantalum spinneret is put into stove, temperature is raised to 500-700 DEG C/insulation 1 hour, vacuum is extracted into 5 × 102,, addition H,
(ratio is 5 to N:1), body of heater cooling water cooling, furnace body temperature drops to less than 100 DEG C, takes out workpiece.
140 DEG C of sulfuric acid/30 minute of tantalum spinneret after ionic nitriding → clear water flushing → deionized water is cleaned by ultrasonic two again
All over// 10 points of each 10 minutes → alcohol ultrasonic cleaning/10 minutes → deionized water of/10 minutes → acetone ultrasonic cleaning ultrasonic cleaning
Clock → drying.After amplifying and being observed under 150 times of measuring microscope without any pollution or foul, with electric welding machine on spinning head
One tantalum foil of weldering is hung on the suspension member in the stove of magnetron sputtering, and the distance regulation suspension member is suitable and distance uniformly shuts stove
Door, spinneret head surface is cleaned with ion gun, and vavuum pump is driven after having cleaned, and it is 5 × 10 that vacuum in stove is evacuated into vacuum-3—8×
10-3Pa, temperature is raised to 180 to 280 DEG C and begins place into acetylene gas, and sputter temperature is 180 DEG C, and sputtering time is 60-80 points
Clock, treats that in-furnace temperature is down to less than 100 DEG C, and workpiece is taken out.
Claims (4)
1. it is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film, it is characterised in that methods described comprises the following steps：
(1) surface of tantalum spinning jet is polished to more than 0.02 μm；
(2) tantalum spinneret after surface is polished is cleaned and dried；
(3) tantalum spinneret after cleaning is detected with microscope, is put into stove if without any pollution, vacuum will be evacuated in stove
Spend is 5 × 102Pa, temperature is raised to 500-700 DEG C, and hydrogen and nitrogen are added after 1-1.5h of insulation, wherein, the volume ratio of hydrogen and nitrogen is
(4.5—5.5):1, with cooling water cooling, tantalum spinneret is taken out when in-furnace temperature is down to below 100 DEG C；
(4) tantalum spinneret of taking-up is cleaned and is dried；
(5) tantalum spinneret after cleaning is detected with microscope, is put into stove if without any pollution, existed with the method for magnetron sputtering
Surface of tantalum spinning jet plates DLC film；The target that plated film is used is acetylene, and plating conditions are as follows：Vacuum is 5 × 10-3—8×
10-3Pa, 180-280 DEG C of temperature, sputtering time is 1-3h；Tantalum spinneret is cooled to less than 100 DEG C after plated film, surface is obtained final product
Plate the tantalum spinneret of DLC film.
2. the method for claim 1, it is characterised in that the cleaning described in step (2) and (4) is after first surface is polished
Tantalum spinneret in the sulfuric acid that concentration is 98%, carry out boiling 25-35min of acid treatment under the conditions of 140 DEG C, then use clear water
Cleaned with deionized water again after flushing, then be cleaned by ultrasonic successively with alcohol, acetone and deionized water in ultrasonic cleaning tank.
3. the method for claim 1, it is characterised in that step (3) and (5) described microscope are to amplify 150 times of survey
Amount microscope.
4. the method for claim 1, it is characterised in that step (5) described sputtering time is 60-80min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611183942.3A CN106756783A (en) | 2016-12-20 | 2016-12-20 | It is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611183942.3A CN106756783A (en) | 2016-12-20 | 2016-12-20 | It is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film |
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| CN106756783A true CN106756783A (en) | 2017-05-31 |
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| CN201611183942.3A Pending CN106756783A (en) | 2016-12-20 | 2016-12-20 | It is a kind of in surface of tantalum spinning jet nitriding and the method for plating DLC film |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380450A (en) * | 2001-04-09 | 2002-11-20 | 北京华宇创新科贸有限责任公司 | Surface treatment method of tantalum sprayer for wet spinning |
| CN1970882A (en) * | 2006-12-13 | 2007-05-30 | 东华大学 | Anti-UV fabric capable of shielding electromagnetic wave and its producing method |
| CN102534614A (en) * | 2011-12-30 | 2012-07-04 | 星弧涂层科技(苏州工业园区)有限公司 | Coating method for DLC (diamond-like carbon) coating on spinning reed and equipment |
-
2016
- 2016-12-20 CN CN201611183942.3A patent/CN106756783A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380450A (en) * | 2001-04-09 | 2002-11-20 | 北京华宇创新科贸有限责任公司 | Surface treatment method of tantalum sprayer for wet spinning |
| CN1970882A (en) * | 2006-12-13 | 2007-05-30 | 东华大学 | Anti-UV fabric capable of shielding electromagnetic wave and its producing method |
| CN102534614A (en) * | 2011-12-30 | 2012-07-04 | 星弧涂层科技(苏州工业园区)有限公司 | Coating method for DLC (diamond-like carbon) coating on spinning reed and equipment |
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