CN104945652B - High hard wear resistant nylon in a kind of surface and preparation method thereof - Google Patents
High hard wear resistant nylon in a kind of surface and preparation method thereof Download PDFInfo
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- CN104945652B CN104945652B CN201510437017.8A CN201510437017A CN104945652B CN 104945652 B CN104945652 B CN 104945652B CN 201510437017 A CN201510437017 A CN 201510437017A CN 104945652 B CN104945652 B CN 104945652B
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Abstract
The present invention discloses high hard wear resistant nylon in a kind of surface and preparation method thereof.The nylon surface has gradient hardening wearing layer；The gradient hardening wearing layer is the Si C cross-linked network layer inorganic carbide layers of ecto-entad；The depth of the gradient hardening wearing layer is 1~6um；Carbon atom percentage composition in the inorganic carbide layer is not less than 95%；The depth of the inorganic carbide layer is 0.5~5um.The method of the present invention forms inorganic carbide layer with argon plasma activated material surface first under vacuum by the way that nylon to be fixed on to the target platform of ion implantation apparatus, then reinjects silicon plasma or silicon, nitrogen plasma form inorganic compounding hardening wearing layer；This method is easy to operate, does not influence the physicalchemical structure of nylon body, and the nylon surface texture obtained after processing is stablized, and case hardness is high, and wear-resisting property is good, and obtained nylon can be widely used for structural load bearing component.
Description
Technical field
The present invention relates to engineering plastic modification technical fields.More particularly, to a kind of system of the high hard wear resistant nylon in surface
Preparation Method.
Background technology
Nylon (Nylon) also known as polyamide, by E.I.Du Pont Company's Tomas Carothers the 1930s (Carothers) and its neck
R＆D team under leading developed, and initially refer in particular to Nylon66, be the fiber that the first is artificial synthesized in the world.With
Afterwards, continuously improving with technique for synthesizing nylon, the commercialization of nylon expand to nylon 6, nylon 11, Buddhist nun from initial nylon66 fiber
Imperial multiple trades mark such as 12, application field also from initial textile fiber extension to structural engineering plastics field, have become
One of most widely used engineering plastics.However, due to having highly polar amido bond in nylon molecules chain, water imbibition is strong, finished product
The dimensional stability of product is poor, and the hydrogen bond in nylon molecules interchain and strand causes the interaction of molecule interchain
It is very strong, can be high than common plastics surface, adhesive force is strong when being contacted with some substances, and friction coefficient is big, causes wear-resisting property insufficient,
Limit its application in the carrying such as bearing, gear, guider, sealing device and joint prosthesis field.
In order to improve the wear-resisting property on nylon surface, currently mainly by increase matrix rigid, addition wearability filler and
The method that is directly modified to article surface is realized.Reinforcing fiber such as glass fibre, carbon fiber, aramid fiber are added in nylon
Fiber etc. can dramatically increase the rigidity of nylon composite materials, improve the case hardness of material, but to composite-material abrasive
Promotion it is limited；And filler such as molybdenum disulfide, carbon black, polytetrafluoroethylene powder, the silicone powder etc. for adding wearability can be carried preferably
The wear-resisting property of high nylon composite materials, but the additive amount of wear resistant filler is larger.Either reinforcing fiber or wear resistant filler
The melt fluidity of composite material can be reduced, the processability of material declines, and is unfavorable for the product of preparation structure complexity.Separately
Outside, it is directly modified for nylon products surface, generally use chemical vapor deposition or Magnetron Sputtered DLC coating (DLC)
Or other wear-resistant coatings are realized, since diamond-like coating (DLC) or other wear-resistant coatings rigidity are stronger, and nylon substrates material
Material rigidity is weaker, causes bonding interface layer internal stress larger, and the binding force of coating and nylon substrates is poor, and it is easy that coating is used for a long time
It is removed from substrate and leads to material failure.
Invention content
It is an object of the present invention to provide a kind of high hard wear resistant nylons in surface.The modification of nylon modified layer is shallow, not shadow
The bulk properties of product, such as tensile strength, impact strength, bending strength and heat distortion temperature physical and chemical performance are rung, it can be wide
It is general to be used for structural load bearing component.
It is another object of the present invention to provide a kind of preparation methods of the high hard wear resistant nylon in surface.This method will not be right
The performance of nylon and its composite body has an impact, and does not influence the processing performance of material；The nylon surface obtained after processing
Stable structure, case hardness is high, and wear-resisting property is good.
To reach above-mentioned first purpose, the present invention uses following technical proposals：
A kind of high hard wear resistant nylon in surface, it is characterised in that：The nylon surface has gradient hardening wearing layer；The ladder
Spend Si-C cross-linked networks layer-inorganic carbide layer that hardening wearing layer is ecto-entad；The depth of the gradient hardening wearing layer is 1
~6um；Carbon atom percentage composition in the inorganic carbide layer is not less than 95%；The depth of the inorganic carbide layer for 0.5~
5um。
Preferably, institute's gradient hardening wearing layer is N-Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.
Preferably, the nylon is selected from nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon bases
Composite material in it is one or more.
To reach above-mentioned second purpose, the present invention uses following technical proposals：
The preparation method of the high hard wear resistant nylon in a kind of surface as described above, using ion implantation apparatus in nylon surface in situ
Build the inorganic hardening wearing layer of gradient.
Preferably, the preparation method includes the following steps：
1) naturally dry is spare after being respectively washed nylon products ethyl alcohol and deionized water totally；
2) nylon obtained in step 1) is placed on ion implantation apparatus target platform, with 4 × 1015~5 × 1017ion/cm2's
Dosage injects argon plasma, and activated nylon strand forms inorganic carbide layer on nylon surface；Entire injection process keeps note
Enter intracavitary pressure not higher than 3 × 10-2Pa, target platform temperature are 80~110 DEG C；After the completion of injection 3 × 10 are not higher than in intracavitary pressure-210~30min is kept under Pa；
3) by nylon processed in step 2), pressure is not higher than 5 × 10 in the cavity in ion implantation apparatus-3Under Pa, with
HIGH-PURITY SILICON is cathode, with 6 × 1015~6 × 1017ion/cm2Dosage injection silicon plasma, it is high hard wear-resisting so as to which surface be made
Nylon.
Preferably, in step 1), the nylon is selected from nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and each
It is one or more in the composite material of kind nylon base.
Preferably, in step 2), the carbon atom percentage composition in the inorganic carbide layer is not less than 95%；The inorganic carbon
The depth for changing layer is 0.5~5um.
Preferably, in step 3), the surface in situ of the high hard wear resistant nylon in obtained surface forms the Si-C of ecto-entad
The gradient hardening wearing layer of cross-linked network layer-inorganic carbide layer；The depth of the gradient hardening wearing layer is 1~6um.
Preferably, in step 3), after the injection of silicon plasma, also comprising being passed through High Purity Nitrogen again, pressure is not in the cavity
Higher than 3 × 10-2Under Pa, by 2 × 1015~6 × 1017ion/cm2The nitrogen plasma injection nylon surface of dosage, so as to be made
The high hard wear resistant nylon in surface；The surface in situ of the high hard wear resistant nylon in the surface forms the N-Si-C cross-linked networks of ecto-entad
The gradient hardening wearing layer of layer-inorganic carbide layer；The depth of the gradient hardening wearing layer is 1~6um.
Preferably, the ion implantation apparatus is All directions ion implantation machine, can be put by radio frequency discharge and cathode vacuum arc
Electricity generates the plasma of multiple gases and solid state component, can apply negative pulse high pressure on target platform, realize to complicated shape system
Part carries out uniform surface ion injection.
In the prior art, for the surface hardening of nylon products and wear-resisting modification, mainly using blending and modifying addition enhancing
The method of fiber and wear resistant filler is realized.But the reinforcing fiber and wear resistant filler of high level need to be generally added, high-content
Filler is unfavorable for the injection molding molding of nylon, it is difficult to the product of preparation structure complexity.In addition it also uses in nylon surface chemistry
Vapor deposition or Magnetron Sputtered DLC coating (DLC) or other wear-resistant coatings carry out direct modification of nylon and realize that hardening is resistance to
Mill.Since diamond-like coating (DLC) or other wear-resistant coatings rigidity are stronger, and nylon substrates material stiffness is weaker, leads to boundary
Face binder course internal stress is larger, and the binding force of coating and nylon substrates is poor, and coating is used for a long time and is easily removed from substrate.The present invention
In view of the deficiencies of the prior art, the method for using plasma injection builds gradient hardening wearing layer in nylon surface in situ, changes
Property layer combines together with substrate nylon, and there is no the situations that modified layer is removed from nylon substrates, belong to product post-processing technology, no
The processing performance of material is influenced, can deficiency of the prior art be overcome with the product of processing structure complexity well, is had non-
Often wide application prospect.
Beneficial effects of the present invention are as follows：
1) technical solution used in the present invention belongs to the post processing surface modification of finished product product, and modified layer is shallow, does not influence product
Bulk properties, such as tensile strength, impact strength, bending strength and heat distortion temperature physical and chemical performance.
2) present invention prepares hardening wearing layer using the method for ion implanting in nylon surface in situ, with the tables such as magnetron sputtering
Face deposition class method of modifying is compared, and modified layer is strong with substrate caking power, and modified layer is not easily to fall off.
3) the high hard wear resistant nylon in prepared surface of the invention can be used for the bearing structures components such as wear-resistant gear.
Specific embodiment
In order to illustrate more clearly of the present invention, with reference to preferred embodiment, the present invention is described further.Ability
Field technique personnel should be appreciated that following specifically described content is illustrative and be not restrictive, this should not be limited with this
The protection domain of invention.
Embodiment 1
6 tablet of nylon after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 4 × 1015ion/cm2
Dosage injection argon plasma, 6 surface of nylon formed inorganic carbide layer.Pressure is 3 in entire injection process holding chamber body
×10-2Pa, target platform temperature are 80 DEG C.After the completion of injection, sample is 3 × 10 in intracavitary pressure-210min is kept under Pa.Then it weighs
The new intracavitary pressure that is evacuated to is 1 × 10-3Pa, with 6 × 1015ion/cm2Dosage injection silicon plasma, it is high hard to obtain surface
Wear-resisting 6 tablet of nylon.High hard wear-resisting 6 planar surface of nylon in the surface has gradient hardening wearing layer, the gradient hardening
Wearing layer is Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.The depth 1um of gradient hardening wearing layer；Wherein, it is inorganic
Carbon atom percentage composition in carburization zone is not less than 95%；The depth of inorganic carbide layer is 0.5um.
Embodiment 2
Nylon66 fiber gear after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 5 × 1017ion/
cm2Dosage injection argon plasma, nylon66 fiber gear surface formed inorganic carbide layer.In entire injection process holding chamber body
Pressure is 1 × 10-2Pa, target platform temperature are 110 DEG C.After the completion of injection, sample is 1 × 10 in intracavitary pressure-2It is kept under Pa
30min.Then it is 1 × 10 to be evacuated to intracavitary pressure again-3Pa, with 6 × 1017ion/cm2Dosage injection silicon plasma,
Obtain the high hard wear-resisting nylon66 fiber gear in surface.The surface of the high hard wear-resisting nylon66 fiber gear in the surface is resistance to gradient hardening
Layer is ground, which is Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.The depth of gradient hardening wearing layer
It spends for 6um；Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%；The depth of inorganic carbide layer is 5um.
Embodiment 3
12 pulley of nylon after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 5 × 1017ion/
cm2Dosage injection argon plasma, 12 pulley surface of nylon formed inorganic carbide layer.In entire injection process holding chamber body
Pressure is 1 × 10-2Pa, target platform temperature are 100 DEG C.After the completion of injection, sample is 1 × 10 in intracavitary pressure-2It is kept under Pa
20min.Then it is 5 × 10 to be evacuated to intracavitary pressure again-3Pa, with 6 × 1016ion/cm2Dosage injection silicon plasma,
Obtain high hard wear-resisting 12 pulley of nylon in surface.The surface of high hard wear-resisting 12 pulley of nylon in the surface is resistance to gradient hardening
Layer is ground, which is Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.The depth of gradient hardening wearing layer
It spends for 6um；Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%；The depth of inorganic carbide layer is 5um.
Embodiment 4
Nylon 11 stick after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 1 × 1016ion/cm2
Dosage injection argon plasma, nylon 11 stick surface formed inorganic carbide layer.Pressure in entire injection process holding chamber body
It is 3 × 10-2Pa, target platform temperature are 80 DEG C.After the completion of injection, sample is 3 × 10 in intracavitary pressure-210min is kept under Pa.So
It is 5 × 10 to be evacuated to intracavitary pressure again afterwards-3Pa, with 6 × 1016ion/cm2Dosage injection silicon plasma, in nylon 11
Stick surface forms the gradient hardening wearing layer of top-down Si-C cross-linked networks layer-inorganic carbide layer, and it is high hard resistance to obtain surface
Grind nylon 11 stick.The depth of the gradient hardening wearing layer of the high hard wear-resisting nylon 11 stick in the surface is 4um；Wherein, inorganic carbon
The carbon atom percentage composition changed in layer is not less than 95%；The depth of inorganic carbide layer is 1um.
Embodiment 5
The compound nylon66 fiber gear of glass hardening after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform,
With 1 × 1016ion/cm2Dosage injection argon plasma, be formed on its surface inorganic carbide layer.Entire injection process holding chamber
Internal pressure is 3 × 10-2Pa, target platform temperature are 90 DEG C.After the completion of injection, sample is 3 × 10 in intracavitary pressure-2It is kept under Pa
10min.Then it is 5 × 10 to be evacuated to intracavitary pressure again-3Pa, with 6 × 1016ion/cm2Dosage injection silicon plasma,
Obtain surface 66 gear of high hard wear resistant nylon.The surface of the high hard wear-resisting nylon66 fiber gear in the surface is wear-resisting with gradient hardening
Layer, the gradient hardening wearing layer are Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.The depth of gradient hardening wearing layer
For 5um；Wherein, the carbon atom percentage composition in inorganic carbide layer is not less than 95%；The depth of inorganic carbide layer is 1um.
Embodiment 6
Nylon 12 after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 1 × 1016ion/cm2's
Dosage injects argon plasma, and inorganic carbide layer is formed on nylon 11 stick surface.Pressure is 3 in entire injection process holding chamber body
×10-2Pa, target platform temperature are 80 DEG C.After the completion of injection, sample is 3 × 10 in intracavitary pressure-210min is kept under Pa.Then it weighs
The new intracavitary pressure that is evacuated to is 5 × 10-3Pa, with 6 × 1016ion/cm2Dosage injection silicon plasma.After the completion of injection,
Sample is 3 × 10 in intracavitary pressure-25min is kept under Pa, is then evacuated to 2.6 × 10-2Pa is passed through High Purity Nitrogen, by 2 ×
1015ion/cm2The nitrogen plasma of dosage is injected into nylon surface, obtains the high hard wear resistant nylon 12 in surface.The surface is high hard
The surface of wear-resisting nylon 12 has gradient hardening wearing layer, which is the netted friendships of N-Si-C of ecto-entad
Join layer-inorganic carbide layer.The depth of gradient hardening wearing layer is 6um；Wherein, the carbon atom percentage composition in inorganic carbide layer is not
Less than 95%；The depth of inorganic carbide layer is 1um.
Embodiment 7
Nylon 1010 idler wheel after fully being cleaned with second alcohol and water is put on ion implantation apparatus target platform, with 1 × 1016ion/
cm2Dosage injection argon plasma, be formed on its surface inorganic carbide layer.Pressure is 3 in entire injection process holding chamber body
×10-2Pa, target platform temperature are 110 DEG C.After the completion of injection, sample is 3 × 10 in intracavitary pressure-210min is kept under Pa.Then
Again it is 1 × 10 to be evacuated to intracavitary pressure-3Pa, with 6 × 1017ion/cm2Dosage injection silicon plasma.Injection is completed
Afterwards, sample is 3 × 10 in intracavitary pressure-25min is kept under Pa, is then evacuated to 2.6 × 10-2Pa is passed through High Purity Nitrogen, by 6
×1017ion/cm2The nitrogen plasma of dosage is injected into nylon 1010 roller surface, obtains the high hard wear resistant nylon nylon in surface
1010 idler wheels.The surface of the high hard wear-resisting nylon 1010 idler wheel in the surface has gradient hardening wearing layer, and the gradient hardening is resistance to
Grind N-Si-C cross-linked networks layer-inorganic carbide layer that layer is ecto-entad.The depth of gradient hardening wearing layer is 6um；Wherein, nothing
Carbon atom percentage composition in machine carburization zone is not less than 95%；The depth of inorganic carbide layer is 1um.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention for those of ordinary skill in the art, may be used also on the basis of the above description
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
The obvious changes or variations that bright technical solution is extended out are still in the row of protection scope of the present invention.
Claims (10)
1. a kind of high hard wear resistant nylon in surface, it is characterised in that：The nylon surface has gradient hardening wearing layer；The gradient
Hardening wearing layer is Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad；The depth of the gradient hardening wearing layer is 1 ~ 6
μm ；Carbon atom percentage composition in the inorganic carbide layer is not less than 95%；The depth of the inorganic carbide layer is 0.5 ~ 5 μm；
The gradient hardening wearing layer is built-up in nylon surface in situ using ion implantation apparatus.
2. a kind of high hard wear resistant nylon in surface according to claim 1, it is characterised in that：The gradient hardening wearing layer is
N-Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad.
3. a kind of high hard wear resistant nylon in surface according to claim 1, it is characterised in that：The nylon is selected from nylon 6, Buddhist nun
Imperial 66, it is one or more in the composite material of nylon 12, nylon 11, nylon 1010 and various nylon bases.
4. a kind of preparation method of the high hard wear resistant nylon in surface as described in any one of claims 1-3, it is characterised in that：Using from
Sub- implanter builds the inorganic hardening wearing layer of gradient in nylon surface in situ.
5. the preparation method of the high hard wear resistant nylon in a kind of surface according to claim 4, which is characterized in that including walking as follows
Suddenly：
1）It is spare that nylon products ethyl alcohol and deionized water are respectively washed clean rear naturally dry；
2）By step 1）In obtain nylon merging ion implantation apparatus target platform on, with 4 × 1015~5×1017 ion/cm2 Dosage
Argon plasma is injected, inorganic carbide layer is formed on nylon surface；Entire injection process keep injection intracavitary pressure not higher than 3 ×
10-2Pa, target platform temperature are 80 ~ 110 DEG C；After the completion of injection 3 × 10 are not higher than in intracavitary pressure-210 ~ 30min is kept under Pa；
3）By step 2 in ion implantation apparatus）In processed nylon in the cavity pressure be not higher than 5 × 10-3 Under Pa, with height
Pure silicon is cathode, with 6 × 1015~6×1017 ion/cm2Dosage injection silicon plasma, so as to which the high hard wear-resisting Buddhist nun in surface be made
Dragon.
6. a kind of preparation method of the high hard wear resistant nylon in surface according to claim 5, it is characterised in that：Step 1）In,
One in composite material of the nylon selected from nylon 6, nylon66 fiber, nylon 12, nylon 11, nylon 1010 and various nylon bases
Kind is a variety of.
7. a kind of preparation method of the high hard wear resistant nylon in surface according to claim 5, it is characterised in that：Step 2）In,
Carbon atom percentage composition in the inorganic carbide layer is not less than 95%；The depth of the inorganic carbide layer is 0.5 ~ 5 μm.
8. a kind of preparation method of the high hard wear resistant nylon in surface according to claim 5, it is characterised in that：Step 3）In,
The surface in situ of the high hard wear resistant nylon in obtained surface forms the ladder of Si-C cross-linked networks layer-inorganic carbide layer of ecto-entad
Spend hardening wearing layer；The depth of the gradient hardening wearing layer is 1 ~ 6 μm.
9. a kind of preparation method of the high hard wear resistant nylon in surface according to claim 5, it is characterised in that：Step 3）In,
After the injection of silicon plasma, also comprising High Purity Nitrogen is passed through again, pressure is not higher than 3 × 10 in the cavity-2Under Pa, by 2 × 1015
~6×1017 ion/cm2The nitrogen plasma injection nylon surface of dosage, so as to which the high hard wear resistant nylon in surface be made；The surface
The gradient hardening of N-Si-C cross-linked networks layer-inorganic carbide layer that the surface in situ of high hard wear resistant nylon forms ecto-entad is wear-resisting
Layer；The depth of the gradient hardening wearing layer is 1 ~ 6 μm.
10. a kind of preparation method of the high hard wear resistant nylon in surface according to claim 5, it is characterised in that：The ion
Implanter is All directions ion implantation machine, can generate multiple gases and solid state component by radio frequency discharge and cathodic vacuum arc discharge
Plasma, negative pulse high pressure can be applied on target platform, realize and uniform surface ion injection is carried out to finished pieces with complex shapes.
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| CN1224772A (en) * | 1998-01-24 | 1999-08-04 | 西南交通大学 | Synthesis of carbon-base film |
| CN100491582C (en) * | 1999-12-23 | 2009-05-27 | 西南交通大学 | Method for forming Tio2-X film on material surface by using plasma immersion ion implantation and use thereof |
| CN103709742A (en) * | 2012-09-29 | 2014-04-09 | 黑龙江鑫达企业集团有限公司 | Modified aramid fiber reinforced PA66 material and preparation method thereof |
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|---|---|---|---|---|
| CN1224772A (en) * | 1998-01-24 | 1999-08-04 | 西南交通大学 | Synthesis of carbon-base film |
| CN100491582C (en) * | 1999-12-23 | 2009-05-27 | 西南交通大学 | Method for forming Tio2-X film on material surface by using plasma immersion ion implantation and use thereof |
| CN103709742A (en) * | 2012-09-29 | 2014-04-09 | 黑龙江鑫达企业集团有限公司 | Modified aramid fiber reinforced PA66 material and preparation method thereof |
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