CN106397804B - A kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces - Google Patents
A kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces Download PDFInfo
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- CN106397804B CN106397804B CN201610879767.5A CN201610879767A CN106397804B CN 106397804 B CN106397804 B CN 106397804B CN 201610879767 A CN201610879767 A CN 201610879767A CN 106397804 B CN106397804 B CN 106397804B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/02—Chemical treatment or coating of shaped articles made of macromolecular substances with solvents, e.g. swelling agents
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
- C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
- C08J2361/16—Condensation polymers of aldehydes or ketones with phenols only of ketones with phenols
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Abstract
The invention discloses the processing methods that a kind of polyether-ether-ketone resin obtains different porous structure surfaces, polyether-ether-ketone (PEEK) material is surface-treated using wet chemistry method, PEEK material is immersed at room temperature in 80%~100% aqueous sulfuric acid 0.5~9 minute, again by PEEK material be immersed in 0 DEG C~100 DEG C water, ethyl alcohol, dimethyl sulfoxide, ethylene glycol, water/alcohol mixed solvent, water/dimethyl sulfoxide mixed solvent or 37~83% aqueous sulfuric acid cleaning agent in, clean 10 minutes.The factors such as concentration, cleaning temperature, the type of cleaning agent and concentration by sulfuric acid when control swelling, obtain the PEEK material of different surface topographies.The present invention can control the through-hole structure on its surface, the size in hole and density and surface through hole pore wall thickness；Simple process, it is at low cost, promote PEEK material in the application in the fields such as electronics, biology and industry.
Description
Technical field
The present invention relates to plastic processing processing technology fields, in particular to a kind of to use wet chemistry method for polyether-ether-ketone
(PEEK) surface treatment method, to obtain the surface of different porous structures.
Background technique
Polyether-ether-ketone (PEEK) is a kind of special engineering plastics, it has outstanding high temperature resistance, mechanical property, resistance toization
Solvent corrosion performance, flame retardant property, radiation-resistant property and good insulation performance are learned, aerospace, automobile, electricity are widely used in
The fields such as sub electrical and health care.The volume resistivity (10 of PEEK14Ω cm) and sheet resistance (1015It is Ω) higher, it is one
The excellent insulating materials of kind.However, higher resistivity limits it in the application of certain electronics industries, such as electricity simultaneously
Magnetic screen.It is the effective way for solving the problems, such as this to PEEK surface metalation.PEEK chemical property is stablized, the knot with metal layer
It is poor with joint efforts, thus material surface is handled, suitable surface topography is obtained, the combination of metal layer and material surface layer is reinforced
It is vital.
PEEK is nontoxic, has excellent chemical solvent resistance energy and radiolucency, and its mechanical property and human body bone
Bone is similar, so PEEK can be used as a kind of excellent biologic graft material.In order to enable PEEK to be effectively combined with bone tissue,
It needs to handle the surface of PEEK, improves the binding force between PEEK and bone tissue.
At industrial circle (and aerospace and automotive field), it is often necessary to glue two pieces or muti-piece PEEK resin
Knot, this needs to improve the binding force between resin, to guarantee work that it can be stable.
Bonding either between the combination or PEEK and PEEK of the combination of metal layer and PEEK, bone tissue and PEEK,
Higher bond strength is to guarantee the key factor of its energy steady operation, and the surface topography of material is the weight for determining binding force power
The factor wanted.Therefore, the surface of PEEK resin is handled, obtains different surface topographies, it can be promoted in electronics, life
The application in the fields such as object and industry.
Summary of the invention
The purpose of the present invention is the shortcomings that overcoming the prior art and deficiency, by using wet chemistry method to PEEK resin
Surface is handled, and different surface topographies is obtained, it is made to be preferably applied for the fields such as electronics, biology and industry.It provides
A kind of simple process, the processing method of PEEK resin surface at low cost, can be used for large-scale industrial production.
The present invention is achieved by following technical solution.
A kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces, has following steps:
(1) oil removing
Polyether-ether-ketone resin material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface；Material is from alkali
Property degreasing fluid in take out after, drying；
(2) concentrated sulfuric acid is swollen
It is 80%~100% that the polyether-ether-ketone resin material for removing the spot on surface is immersed volume fraction at room temperature
In aqueous sulfuric acid, impregnate 0.1~30 minute；
(3) swollen material is cleaned
Polyether-ether-ketone resin material after swelling is immersed in the cleaning agent of opposed polarity, scavenging period is 10 minutes,
Cleaning agent temperature is 0 DEG C~100 DEG C；
The cleaning agent is water, ethyl alcohol, dimethyl sulfoxide, ethylene glycol, water/alcohol mixed solvent, water/dimethyl sulfoxide are mixed
The aqueous sulfuric acid that bonding solvent and volume fraction are 37~83%；The water is distilled water or tap water；
(4) secondary cleaning material
When the cleaning agent of step (3) is non-aqueous cleaning agent, need to carry out secondary cleaning to material；
Material after step (3) cleaning is immersed in tap water at room temperature 10 minutes, is then dried up, is made not
With the polyether-ether-ketone resin on porous structure surface.
The conventional alkaline degreasing fluid of the step (1) are as follows: sodium hydroxide 25g/L, natrium carbonicum calcinatum 40g/L, sodium phosphate
35g/L, additional OP series emulsifier 2ml/L.
The present invention is handled by surface of the wet chemistry method to PEEK resin, is obtained different surface topographies, is made it
It is preferably applied for the fields such as electronics, biology and industry.Present invention process is simple, at low cost, to can be used for large-scale industry raw
The processing method of the PEEK resin surface of production.
Detailed description of the invention
Fig. 1 is the stereoscan photograph of gained PEEK surface topography after embodiment 1 is handled；
Fig. 2 is the stereoscan photograph of gained PEEK surface topography after embodiment 2 is handled；
Fig. 3 is the stereoscan photograph of gained PEEK surface topography after embodiment 3 is handled；
Fig. 4 is the stereoscan photograph of gained PEEK surface topography after embodiment 4 is handled；
Fig. 5 is the stereoscan photograph of gained PEEK surface topography after embodiment 5 is handled；
Fig. 6 is the stereoscan photograph of gained PEEK surface topography after embodiment 6 is handled；
Fig. 7 is the stereoscan photograph of gained PEEK surface topography after embodiment 7 is handled；
Fig. 8 is the stereoscan photograph of gained PEEK surface topography after embodiment 8 is handled；
Fig. 9 is the stereoscan photograph of gained PEEK surface topography after embodiment 9 is handled；
Figure 10 is the stereoscan photograph of gained PEEK surface topography after embodiment 10 is handled；
Figure 11 is the stereoscan photograph of gained PEEK surface topography after embodiment 11 is handled；
Figure 12 is the stereoscan photograph of gained PEEK surface topography after embodiment 12 is handled；
Figure 13 is the stereoscan photograph of gained PEEK surface topography after embodiment 13 is handled；
Figure 14 is the stereoscan photograph of gained PEEK surface topography after embodiment 14 is handled；
Figure 15 is the stereoscan photograph of gained PEEK surface topography after embodiment 15 is handled；
Figure 16 is the stereoscan photograph of gained PEEK surface topography after embodiment 16 is handled；
Figure 17 is the stereoscan photograph of gained PEEK surface topography after embodiment 17 is handled；
Figure 18 is the stereoscan photograph of gained PEEK surface topography after embodiment 18 is handled；
Figure 19 is the stereoscan photograph of gained PEEK surface topography after embodiment 19 is handled；
Figure 20 is the stereoscan photograph of gained PEEK surface topography after embodiment 20 is handled；
Figure 21 is the stereoscan photograph of gained PEEK surface topography after embodiment 21 is handled；
Figure 22 is the stereoscan photograph of the PEEK surface topography after oil removing.
Specific embodiment
The present invention is described in more detail in the following with reference to the drawings and specific embodiments, but the present invention is not restricted to these implement
Example.
Embodiment 1:
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 88% at room temperature, at swelling
Reason 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 2:
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 94% at room temperature, at swelling
Reason 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 3
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 97% at room temperature, at swelling
Reason 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 4
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 5
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in ethyl alcohol at room temperature, the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 6
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in dimethyl sulfoxide at room temperature, the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 7
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in distilled water/alcohol mixed solvent at room temperature, distilled water/ethyl alcohol volume point
For number than being 3/1, the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 8
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in distilled water/alcohol mixed solvent at room temperature, distilled water/ethyl alcohol volume point
For number than being 1/1, the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 9
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in distilled water/alcohol mixed solvent at room temperature, distilled water/ethyl alcohol volume point
For number than being 1/3, the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 10
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed into distilled water/dimethyl sulfoxide in the mixed solvent at room temperature, distilled water/diformazan
Base sulfoxide Volume fraction is 3/1, and the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 11
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed into distilled water/dimethyl sulfoxide in the mixed solvent at room temperature, distilled water/diformazan
Base sulfoxide Volume fraction is 1/1, and the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 12
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed into distilled water/dimethyl sulfoxide in the mixed solvent at room temperature, distilled water/diformazan
Base sulfoxide Volume fraction is 1/3, and the time is 10 minutes.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 13
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in the aqueous sulfuric acid that volume fraction at room temperature is 83%, the time is 10 points
Clock.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 14
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in the aqueous sulfuric acid that volume fraction at room temperature is 64%, the time is 10 points
Clock.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 15
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in the aqueous sulfuric acid that volume fraction at room temperature is 37%, the time is 10 points
Clock.
(4) secondary cleaning material
It immerses the material in tap water at room temperature 10 minutes, then dries up material with hair dryer.
Embodiment 16
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in 0 DEG C of tap water, the time is 10 minutes, then dries up material with hair dryer
Material.
Embodiment 17
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in 60 DEG C of tap water, the time is 10 minutes, then dries up material with hair dryer
Material.
Embodiment 18
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 0.5 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in 100 DEG C of tap water, the time is 10 minutes, then dries up material with hair dryer
Material.
Embodiment 19
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 1 minute.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 20
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 3 minutes.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
Embodiment 21
(1) oil removing
PEEK material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface.After being taken out in oil removing, use
Hair dryer dries up material.
(2) concentrated sulfuric acid is swollen
The PEEK material for removing the spot on surface is immersed in the concentrated sulfuric acid that volume fraction is 100% at room temperature, swelling
Processing 9 minutes.
(3) swollen material is cleaned
PEEK material after swelling is immersed in tap water at room temperature, the time is 10 minutes, is then dried up with hair dryer
Material.
See Table 1 for details for the main technologic parameters of the specific embodiment of the invention.
Table 1
Specific embodiment is described as follows below by attached drawing:
The SEM picture of PEEK natural surface before Figure 22 is swelling treatment, material surface is smooth, fine and close, exists on surface
Some moldings and the streak left when demoulding.For embodiment 1,2,3 and 4, when the sulfuric acid treatment for being 88% with volume fraction
When PEEK, the streak structure on raw material surface disappears, and material surface becomes more smooth, fine and close (Fig. 1).When the volume point of sulfuric acid
When number is 94%, there is a small amount of, nanoscale, isolated aperture (Fig. 2) in material surface.Further by the volume of sulfuric acid point
Number is increased to 97%, and the micropore (Fig. 3) of a large amount of perforation occurs in material surface.At the sulfuric acid for being 100% with volume fraction
When managing PEEK, equally there is the micropore (Fig. 4) of a large amount of perforation in material surface, but with shape obtained by the sulfuric acid with 96.8%
Looks are compared, and the micropore on surface is more, closeer, and the hole wall of through hole attenuates.
For embodiment 5 and 6, when being cleaned in the ban with ethyl alcohol, the surface PEEK shows a small amount of isolated hole (Fig. 5), this
When surface pore density very little.When first being cleaned with dimethyl sulfoxide after swelling, the surface PEEK shows more hole knot
Structure (Fig. 6), the quantity of surface holes is more, and hole wall is thicker, and the depth in hole is shallower, and many holes are in open state.
For embodiment 7,8 and 9, when water/alcohol ratio is 3/1, as shown in fig. 7, material surface equally occur it is a large amount of,
The micropore of perforation, gained surface topography is similar when pattern is cleaned with tap water.When water/alcohol ratio is 1/1, such as Fig. 8, surface is same
Sample shows through-hole structure, but the density of surface holes decreases, hole wall thickening.When water/alcohol ratio is 1/3, such as Fig. 9,
The surface PEEK shows isolated hole configurations, and many holes are shallower, and opening-like.
For embodiment 10,11 and 12, when water/sulfone ratio is 3/1, as shown in Figure 10, material surface equally occur compared with
Shallow perforation micropore, but the distribution of through hole and uneven.When water/sulfone ratio is 1/1, such as Figure 11, surface equally shows
The density of through-hole structure, surface holes increases, and is evenly distributed.When water/sulfone ratio is 1/3, such as Figure 12, the density of surface through hole
It is reduced, the size in hole and is unevenly distributed.
For embodiment 13,14 and 15, when being rinsed again with tap water with 83.0% sulfuric acid cleaned in the ban, the surface PEEK is in
Reveal a small amount of isolated hole configurations (Figure 13).However, (figure when being rinsed again with tap water with 63.5% sulfuric acid cleaned in the ban
14), surface shows through-hole structure, and hole wall is thicker.(figure when being rinsed again with tap water with 37.3% sulfuric acid cleaned in the ban
15), surface is similarly through-hole structure, but compared with figure 14, surface via densities increase, and hole wall attenuates.Obviously, when with sulfuric acid
When solution makees cleaning agent, reducing with sulfuric acid concentration from isolated hole becomes through hole, and the quantity and density in hole increase, and hole wall attenuates.
For embodiment 16,17 and 18, as shown in figure 16 in 0 DEG C of the resulting surface topography of tap water immersion, surface is in
Now penetrate through pore structure.Compared with the material impregnated at room temperature (Fig. 4), surface through-hole becomes closeer, and hole wall becomes thinner.Work as leaching
When entering in 60 DEG C of tap water (Figure 17), surface is perforation pore structure, compared with the material impregnated at room temperature (Fig. 4), hole
Variable density is little, but the thickness of hole wall increased.When in the tap water for immersing 100 DEG C (Figure 18), surface is still through-hole
Structure, but the density in hole reduces, pore wall thickness obviously increases.Obviously, it is increased with tap water temperature when cleaning, surface through-hole
Density reduces, and hole wall thickens.
For embodiment 19,20 and 21, when the sulfuric acid treatment PEEK that volume fraction is 100%, the variation pair of time is handled
The surface topography of material influences less, and material surface presents the micropore of a large amount of perforation, hole wall it is thin (Figure 19,20,
21)。
Claims (2)
1. a kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces, there are following steps:
(1) oil removing
Polyether-ether-ketone resin material is immersed in conventional alkaline degreasing fluid, to remove the spot of material surface；Material is removed from alkalinity
After being taken out in oil liquid, drying；
(2) concentrated sulfuric acid is swollen
The polyether-ether-ketone resin material for removing the spot on surface is immersed into the sulfuric acid that volume fraction is 80%~100% at room temperature
In aqueous solution, impregnate 0.5~9 minute；
(3) swollen material is cleaned
Polyether-ether-ketone resin material after swelling is immersed in the cleaning agent of opposed polarity, scavenging period is 10 minutes, cleaning
Agent temperature is 0 DEG C~100 DEG C；
The cleaning agent is water, ethyl alcohol, dimethyl sulfoxide, ethylene glycol, water/alcohol mixed solvent, water/dimethyl sulfoxide mixing are molten
The aqueous sulfuric acid that agent or volume fraction are 37~83%；The water is distilled water or tap water；
(4) secondary cleaning material
When the cleaning agent of step (3) is non-aqueous cleaning agent, need to carry out secondary cleaning to material；
Material after step (3) cleaning is immersed in tap water at room temperature 10 minutes, is then dried up, is made different more
The polyether-ether-ketone resin on pore structure surface.
2. a kind of polyether-ether-ketone resin according to claim 1 obtains the processing method on different porous structure surfaces, special
Sign is, the conventional alkaline degreasing fluid of the step (1) are as follows: sodium hydroxide 25g/L, natrium carbonicum calcinatum 40g/L, sodium phosphate 35g/
L, additional OP series emulsifier 2ml/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610879767.5A CN106397804B (en) | 2016-09-30 | 2016-09-30 | A kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610879767.5A CN106397804B (en) | 2016-09-30 | 2016-09-30 | A kind of polyether-ether-ketone resin obtains the processing method on different porous structure surfaces |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106397804A CN106397804A (en) | 2017-02-15 |
| CN106397804B true CN106397804B (en) | 2019-02-15 |
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| CN109364296B (en) * | 2018-10-23 | 2022-04-22 | 大连理工大学 | Surface-modified polyaryl ether bone implant material containing phthalazinone structure and preparation method thereof |
| CN112808688B (en) * | 2021-01-05 | 2023-04-11 | 上海理工大学 | Method for cleaning small-size pore powder of PEEK material 3D printing product |
| CN116041901B (en) * | 2022-12-28 | 2023-08-04 | 江苏君华特种工程塑料制品有限公司 | PEEK alloy and preparation method thereof |
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| CN103191468A (en) * | 2013-04-19 | 2013-07-10 | 深圳大学 | Human bone substitute material and preparation method thereof |
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| CN103191468A (en) * | 2013-04-19 | 2013-07-10 | 深圳大学 | Human bone substitute material and preparation method thereof |
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| Title |
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| "Cytocompatibility, osseointegration, and bioactivity of three-dimensional porous and nanostructured network on polyetheretherketone";Ying Zhao et al.;《Biomaterials》;20130914;第34卷;第9264-9277页 |
| "Influence of sulfur content on bone formation and antibacterial ability of sulfonated PEEK";Liping Ouyang et al.;《Biomaterials》;20160106;第83卷;第115-126页 |
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