CN108441925A - A kind of New Anodizing Process preprocess method - Google Patents
A kind of New Anodizing Process preprocess method Download PDFInfo
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- CN108441925A CN108441925A CN201810350500.6A CN201810350500A CN108441925A CN 108441925 A CN108441925 A CN 108441925A CN 201810350500 A CN201810350500 A CN 201810350500A CN 108441925 A CN108441925 A CN 108441925A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/26—Anodisation of refractory metals or alloys based thereon
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Abstract
A kind of Novel anode Pretreatment Methods of the present invention are related to the processing method of bio-medical material, especially prepare the surface preparation before titanium or titanium alloy anodic oxidation.Including carrying out dry ice particles spray treatment to matrix surface；1‑1）Dry ice particles are handled, changes the size of dry ice particles or changes simultaneously the size and shape of dry ice particles；1‑2）Spray treatment is carried out to matrix surface；To achieve the purpose that purification, roughening pretreating surface.The method of the present invention improves existing dry ice blasting cleaning, instead of existing sandblasting/centrifugation grinding technics, it might even be possible to omit activation procedure；After being handled using dry ice particles jet cleaning technology, it is found that the quantity for the abrasive grain fragment for remaining in matrix surface substantially reduces, interface pollution is basically eliminated.Reaching purification, roughening matrix surface simultaneously, interface is not in apparent abrasive grain fragment residual, greatly reduces secondary interface pollution；Improve film layer interface quality, bond strength and service life.
Description
Technical field
A kind of Novel anode Pretreatment Methods of the present invention are related to the processing method of bio-medical material, especially prepare
Surface preparation before titanium or titanium alloy anodic oxidation.
Background technology
Titanium or titanium alloy is widely used as bio-medical material application due to good biocompatibility, is especially being planted
Enter object field.Higher biocompatibility spontaneous one layer of stabilization of generation and can have in use derived from titanium or titanium alloy
Oxidation film protective to a certain degree.In addition, consider that titanium or titanium alloy density is about 4.5 grams per cubic centimeter from structural point,
The only half of steel.Its specific strength is high simultaneously, and specific stiffness is high, therefore titanium or titanium alloy is the first choice as implant material at present
Material.
For the processing of current medical instrument field implantation material product, majority of case is needed to medical titanium or titanium alloy
Carry out anodized.Purpose has four：First, improving the wearability of titanium or titanium alloy, reduces titanium or titanium alloy and using process
In abrasion.Second is that improving the corrosion resistance of titanium or titanium alloy, the corrosion rate of titanium or titanium alloy in use is reduced.Three
Be using newly-generated oxidation film as diffusion barrier layer, weaken titanium alloy in certain toxic metal ions dissolution, such as vanadium from
Son, to reduce cytotoxicity.Fourth, the oxidation film of different colours is also used as in art quick and precisely distinguishing different implantation groups
The means of part.As it can be seen that using anode oxidation process to titanium or titanium alloy carry out coloring treatment, can reach material functionality with
The harmony of aesthetics.
Before carrying out anodized to medical titanium or titanium alloy, need to pre-process its surface.Anodic oxygen
Metaplasia at the bond strength of oxidation film, the surface quality of matrix is closely related before film thickness range and anodic oxidation.Therefore anode
Surface preparation before oxidation is highly important process in anodizing technology.
Three purification, roughening and activation links are generally comprised to the pretreatment of metallic matrix before anodic oxidation.Purified treatment
Refer to greasy dirt, oxide, paint and other dirts for removing workpiece and waiting for anodized surface, at present in anodic oxidation pretreatment
The purifying treatment method used be mainly electrochemical deoiling, vapour degreasing, steam purge, pickling, ultrasonic cleaning, centrifugation grinding with
And the methods of magnetic grinding.And roughening treatment is then to make purified matrix be formed by relevant processing to have particular surface thick
The purpose of implantation material biocompatibility is improved to reach the contact area of increase artificial implantation-people's bone in the surface of rugosity.Often
Roughening treatment has sandblasting（Including dry blasting and wet abrasive blasting）, water flow jet, machining, laser ablation and chemical attack etc.
Method.Wherein, sandblasting pretreatment is easy to operate, and applicability is wide, therefore is applied the most generally in current medical implant industry
Anodic oxidation front surface preprocess method.Activation process is also known as surface adjustment, and effect is to eliminate physics existing for workpiece surface
Or the inhomogenous influence that film forming procedure is brought of chemistry.It usually utilizes specific acid or aqueous slkali by workpiece etch, makes work
Part exposes uniform fresh metal surface, improves matrix surface chemical potential.
Preprocess method used in current medical instrument industry generally uses following two approach.One is using dry blasting
Method, then carry out acid activation process.Second is that using centrifugation grinding and/or the method for magnetic grinding, acid is then carried out
Activation process.
Both pretreatment approach are attained by the purpose of purification, roughening, activation, but there are one common defects.Cause
Abrasive material remains, and pollutes matrix surface.The principle of sandblasting is to be accelerated abrasive material using high pressure draught, is then ejected into matrix surface,
By the erosion effect roughening matrix surface of abrasive grain, and play the role of purification and activation to a certain extent.Centrifugation grinding
Principle is the rotation using revolution and negative direction, makes abrasive material that relative motion occur with workpiece, to generate abrasive material to matrix surface
Micro-cutting, to achieve the purpose that purify workpiece surface.The two essence is identical, is all to reach net using the micro-cutting of exotic
Change, the effect of roughening matrix surface.Meanwhile the two also has identical defect.It can all generate dust and noise pollution；It handles thin
When wall pieces, the problems such as be easy to causeing part deformation.Most significant problem is that matrix surface is easy the presence of remaining abrasive grain among these.Especially
It is for the preferable matrix of the plasticity such as titanium or titanium alloy, stainless steel, aluminium alloy, and abrasive grain is easy embedded base when sandblasting/centrifugation is ground
Body, it is difficult to remove.
This abrasive grain residual effect film performance, specifically includes following defect：
1）Matrix surface integrality is reduced, Particulate Inclusion is substantially the introduction of, causes interface pollution.
The local failure homogeneity of matrix surface, local cell karyogenesis and long senior general generate big brilliant different from normal surface
Body, and fine grain compact tissue heterogeneous.
2）Reduce matrix and the interface bond strength of film layer.
3）The stress field of film layer/basal body interface is impacted, to cause local film layer to fall off.
4）The a series of physical performance such as conduction, heat conduction is impacted, this is buried under the internal environment of human body complexity
The seed of unknowable harm occurs.
Blasting treatment has two kinds of wet abrasive blasting and dry blasting, is usually dry blasting work for the pretreated technique of anodic oxidation
Skill.The principle of dry blasting is to be accelerated abrasive material using high pressure draught, is then ejected into matrix surface, is acted on by the erosion of abrasive grain
It is roughened matrix surface.The type of abrasive material generally comprises aluminium oxide, silicon carbide, the fragile materials such as iron sand.
Dry blasting causes the concrete principle of roughing in surface to be：Abrasive grain promotes matrix surface to send out by high velocity impact matrix surface
Raw plastic deformation, the effect for gathering around angular particle are similar to chisel, dig out the irregular pattern on surface.In fact, according to
The observation of Griffith, there are mainly two types of patterns with matrix surface effect for abrasive grain.The first pattern is by possessing the abrasive grain of the top of the horn
Direct shock, pit is generated, while at edge with a degree of crimping.Often corner angle are clearly demarcated pit, and hit
The shape of particle is similar.The plastic deformation for being formed as matrix surface of pit and the internal material next to matrix surface
Flexible deformation comprehensive function.Here be referred to as pit type deformation pattern.Second of pattern Impact Abrasive high speed
It hits matrix surface and micromachined goes out periphery with larger lip crimping or end with larger bow type crimping
Pit.At this moment the sharp edge of abrasive grain is deeply cut inside parent metal, will be cut out while cut out larger fresh surface
Metal stacks to periphery and is not subjected to the surface hit.The deformed shape that matrix surface generates after this shock and the first pattern
The pit of generation is compared, and length is often longer, and centainly curved occurs while totally keeping sharp in tangent line.We
Here it is referred to as indentation type deformation pattern.
Either pit type deformation pattern or indentation type deformation pattern are likely to cause adhering to, being embedding for sand grains fragment
Enter.
There are two the reason of abrasive grain attachment, embedded matrix.
First, abrasive grain is driven by compressed air occurs high-speed impact in matrix surface.When hitting, due to the elasticity of matrix
Modulus and plastic deformation ability will be far superior to abrasive grain itself.Therefore, when abrasive grain high-speed impact, although most of abrasive grains can
Rebound, but small part abrasive grain can be crushed, and while most of fragment rebounds away, partial piece directly adheres to, is embedded
Inside matrix surface, no longer rebound away.
Second is that abrasive grain is driven by compressed air occurs high-speed impact in matrix surface.Since abrasive grain itself belongs to brittleness material
Material, therefore there is the phenomenon that a part of fragment is detached from its abrasive grain ontology when hitting in many abrasive grains.Sometimes abrasive grain ontology and one
Morcelling piece can leave from matrix surface rebound, but has small part fragment and remain in matrix surface.Then next
When abrasive grain hits matrix surface, impingement position is on the remnants abrasive grain fragments, to be embedded into inside matrix surface.This
The probability that kind situation occurs is more compared to the first situation.
It can be seen that although dry blasting processing can play the role of purification, roughening matrix surface, after dry blasting processing
It easy tos produce broken abrasive grain fragment and remains in matrix surface, which often exists with state that is embedded or adhering to, it is difficult to
Removal, to form new surface contamination.If handled by subsequent anode oxidation membrane, these surface contaminations are finally still
It can be present in film layer/basal body interface, cause interface inclusion.Or cause local film thickness very thin by even zero, cause film layer uneven.
Therefore, abrasive material residual destroys the surface integrity of matrix, introduces Particulate Inclusion, causes interface pollution.Gdna contamination is brilliant
Karyogenesis and long senior general may be not easy forming core or generate big crystal different from normal surface, and fine grain compact tissue heterogeneous.
Reduce the bond strength of matrix and film layer.The stress field of film layer/basal body interface is impacted, to cause local film layer de-
It falls.The a series of physical performance such as conduction, heat conduction is impacted, possible generation is buried in the internal environment of human body complexity can not
Know the seed of harm.Therefore, abrasive material residual rate is reduced, interface pollution is improved, it is significant.
Dry ice particles cleaning mainly impacts matrix surface using dry ice particles, passes through collision effect（Including momentum transfer,
Effect of micro-explosion and gas lift effect）, thermal shock, transient state liquid CO 2 dissolution etc. realize the cleaning to surface.It touches
The effect of hitting refers to that high pressure gas carrying dry ice particles act on matrix surface, and particle collides with surface, dry ice particles and table
Extraneous contamination or impurity particle the generation momentum transfer with surface in face, makes surface particles that adhesion strength be overcome to be desorbed（This is viscous
Attached power is mainly Van der Waals force in dry environment）.Meanwhile dry ice particles are caused in the transient evaporation of high-speed impact matrix surface
It is gas so that the dry ice particles of solid is distilled rapidly, and the volume of dry ice particles expands nearly thousand times within some thousandths of second, impacting
Point causes miniature explosion, makes pollutant or exogenous impurity avalanche.Also, the effect of lifting of the gas caused by miniature explosion, also can will be all
Pollutant or exogenous impurity the purging stripping on side.High wind-warm syndrome refers to sample surface temperature in dry ice particles course of injection
Drastically decline, due to high wind-warm syndrome（Its effect degree is influenced by the thermal property of matrix, pollutant）Cause to adhere to impurity mistake
Go elasticity, shrink, crack, is broken, being desorbed etc., it is final to remove.Matrix and external contaminant, impurity coefficient of thermal expansion not
With causing matrix surface and the binding force of pollutant, impurity to weaken, the non-uniform shrinkage in layer of contaminants causes fragment to generate, from
And eventually lead to layer separation.Transient state liquid CO 2 dissolution refers to dry ice particles in the elastic collision process with surface
In, the pressure of contact surface, temperature reach three phase point, and carbon dioxide liquefies on the contact surface, can play the role of solvent, nonpolarity
Organic matter dissolves rapidly.Dry ice particles are detached from from surface rebound, take away impurity.But due to dry ice particles cleaning pressure and
Dry ice particles are smaller, and the surface roughness reached also tends to smaller, and the requirement of roughness needed for product is not achieved.
Invention content
The purpose of the present invention is preprocess methods before a kind of Novel anode of place oxidation against the above deficiency, instead of previous
Sandblasting/centrifugation grinding method carries out dry ice particles cleaning, is mingled with residual volume to play significant decrease film layer-basal body interface
Effect.
The present invention takes following technical scheme to realize：
A kind of preceding preprocess method of Novel anode oxidation, includes the following steps,
1）Dry ice particles spray treatment is carried out to matrix surface
1-1）Dry ice particles are handled, changes the size of dry ice particles or changes simultaneously the size and shape of dry ice particles；
Dry ice particles are processed as by cylinder, hexahedron or the octahedral bodily form using manufacture dry ice equipment, increase single dry ice particles
Cutting face；
1-2）Spray treatment is carried out to matrix surface；
Using spraying equipment, dry ice particles injection is carried out to matrix surface by suction-type spray regime or forced spray regime
Processing；Compressed air pressure ranging from 0.1~1.5 megapascal when injection；To the mesh for reaching purification, being roughened pretreating surface
's；
2）To passing through step 1）Matrix surface after spray treatment carries out activation process；
Workpiece surface is activated using acid or alkaline activation liquid, achievees the purpose that activating surface.
Step 2）In activating solution can select single acid solution, such as nitric acid or combination of acidic solution, it is a certain amount of
Nitric acid match a certain amount of hydrofluoric acid；The alkaline solution of strong oxidizing property, such as KMnO can also be used4Solution.
The mixture of nitric acid and hydrofluoric acid, ratio range are：100 milliliters of nitric acid（Concentration：65-68%）：5-20 milliliters of hydrogen
Fluoric acid（Concentration >=40%）.
Step 2）In soak time be 10~30 seconds, ranging from 20~50 DEG C of tank liquor temperature.
Optimal soak time is combined as 15 seconds and 25 DEG C with tank liquor temperature.
Step 1-1）Single dry ice particles size range that treated（The full-size of individual particle）It is 5-15 millimeters, spray
When penetrating dry ice range of flow be 10-60 kilograms per hour.
Single dry ice particles size（The full-size of individual particle）Optimal is not less than 10 millimeters.
When injection dry ice flow it is optimal be 40 kilograms per hour.
Step 1-2）In spraying equipment may be used spray gun, lance tube uses Lavalle mouth structure.
Ranging from 13-20 millimeters of the nozzle diameter of spray gun.
The distance range of spray gun to matrix is 15-50 millimeters；The distance of optimal spray gun to matrix is 25 millimeters.
Preprocess method can also apply the cleaning after roughening treatment technique before Novel anode oxidation of the present invention
Technique is not merely limited to the alternate process instead of interface pollution caused by sandblasting.
The present invention is as preprocess method before a kind of anodic oxidation, in some cases, step 2）It is not essential, that is, has
When can be omitted step 2）" activation process is carried out to matrix surface ".Pass through collision effect（Including momentum transfer, effect of micro-explosion with
And gas lifts effect）, thermal shock, transient state liquid CO 2 dissolution etc. realize the cleaning to surface, high speed injection it is dry
Ice particle can also take away a part of titanium alloy substrate material, while adjusting matrix surface while taking away external contaminant
Microscopic appearance.It is final to make to wait for that the matrix exposing chemical potential of anodic oxidation is higher, the uniform fresh material surface of microscopic appearance（This with
The purpose of activation step is identical）.Therefore, in some cases, only by step 1）" dry ice particles injection is carried out to matrix surface
Processing ", to omit step 2）" activation process is carried out to matrix surface ".
By the method for the present invention treated wait for anodic oxidation basal body interface exotic pollute significantly reduce.
The method of the present invention grinds caused interface pollution to eliminate sandblasting/centrifugation, improves anode oxidation membrane quality,
Existing dry ice blasting process is improved, instead of existing sandblasting/centrifugation grinding technics, it might even be possible to omit activation procedure；It is adopting
After being handled with dry ice particles jet cleaning technology, it is found that the quantity for the abrasive grain fragment for remaining in matrix surface drops significantly
Low, interface pollution is basically eliminated.Anodic oxidation preprocess method provided by the invention is reaching purification, roughening matrix surface
While, interface is not in apparent abrasive grain fragment residual, greatly reduces secondary interface pollution；The boundary of film layer can be improved
Face quality, bond strength and service life.
Description of the drawings
Below with reference to attached drawing, the invention will be further described：
Fig. 1 is typical energy spectrum analysis photo in specific embodiment after A groups test piece anodized.
Fig. 2 is then film layer/basal body interface that C groups spray after dry ice blasting in specific embodiment.10 be film layer,
20 be matrix, and 30 be interface, and 40 be remaining abrasive grain fragment.
Fig. 3 is in specific embodiment, then film layer/basal body interface of spraying after D group dry blastings.10 be film layer, and 20 be base
Body, 30 be interface, and 40 be remaining abrasive grain fragment.
Specific implementation mode
It will illustrate the process of the method for the present invention realization by specific embodiment below, and pass through the comparative analysis present invention's
Effect.
Specific embodiment one,
The embodiment discloses one kind and being used for the pretreated technique of anodic oxidation, and substantially steps are as follows：
1）The test piece matrix surface for treating anodic oxidation carries out oil removing grease removal processing；
2）Dry ice blasting roughening treatment is carried out to test piece；
3）Particular solution activation process is carried out to test piece；
4）Specific anodized is carried out to test piece.
Dry blasting roughening causes remaining abrasive grain fragment in the adhering to of matrix surface, is embedded in, and causes interface pollution.It is adopted to understand
Purification, roughening effect with dry ice particles injection to test piece, the present embodiment are compared using conventional dry blasting method.
Conventional process substantially steps are as follows：
1）The test piece matrix surface for treating anodic oxidation carries out oil removing grease removal cleaning；
2）Dry blasting roughening treatment is carried out to test piece；
3）Particular solution activation process is carried out to test piece；
4）Specific anodized is carried out to test piece.
The concrete operation step of entire embodiment is as follows：
1）Matrix is the TA3 titaniums disk totally 10 of 25 millimeters of diameter, 2 millimeters of thickness, and TA3 ingredients see the table below 1（Table 1 is tool
TA3 materials are after oil removing grease removal cleaning in body embodiment, EDAX results that surface face is swept）.
2）All 10 test pieces have carried out acetone ultrasonic cleaning first before roughening treatment, reach the mesh of oil removing grease removal
's.
3）Dry blasting roughening treatment is carried out to wherein 5 test pieces.Dry spray is carried out to it using 220 mesh white alumina abrasive grains
Sand.Dry blasting compressed air pressure is 0.4 megapascal, and sandblasting distance is 250 millimeters, and sandblasting angle is 90 degree, and overlapping rate is 50%,
Sandblasting pass is 3 times.
Dry ice particles injection roughening is carried out to other 5 test pieces.Dry ice is hexahedron dry ice particles, individual particle maximum ruler
Very little to be not less than 10 millimeters, per hour for 40 kilograms, dry ice spray gun to matrix distance is 25 millimeters to the flow of dry ice particles.
4）Above-mentioned all 10 test pieces are activated.Activating solution uses nitric acid, the hydrofluoric acid mixture of special formulation, living
Change 15 seconds time, tank liquor temperature is 25 DEG C.
5）Anodized is carried out at the same time using specific tooling to above-mentioned all 10 test pieces, altering anodization parameters are specific
The electrolyte of formula, 110 volts of voltage, anodizing time 15 seconds, electrolyte temperature are 25 DEG C.
1 TA3 energy spectrum analysis ingredients of table
Above-mentioned 2 kinds of test pieces are marked.5 test pieces after label lives through sandblasting roughening and activates are A group test pieces.Label warp
5 test pieces gone through after dry ice particles injection are B group test pieces.
Surface scan is carried out to strip using energy depressive spectroscopy, the results showed that there are 2.29% mass percents for the test piece of A groups
Aluminium, B group test pieces do not detect aluminium content.5 strip faces of A groups sweep energy spectrum analysis initial data and are shown in Table 2, Sjffle dE A typical spectrum
Figure is shown in Fig. 1.It can be seen that A groups strip is because there are white alumina remnants abrasive materials, therefore present in energy spectrum analysis micro
Aluminium content.And B groups are because use dry ice particles spray technology to replace traditional blasting craft, therefore in energy spectrum analysis simultaneously
Aluminium element is not found.
2 A group test piece energy spectrum analysis ingredients of table
Specific embodiment two,
The embodiment discloses one kind and being used for the pretreated technique of anodic oxidation, and substantially steps are as follows：
1）The test piece matrix surface for treating anodic oxidation carries out oil removing grease removal processing；
2）Dry ice blasting roughening treatment is carried out to test piece；
3）Supersonic flame spraying processing is carried out to test piece.
Dry blasting roughening causes remaining abrasive grain fragment in the adhering to of matrix surface, is embedded in, and causes interface pollution.It is adopted to understand
Purification, roughening effect with dry ice particles injection to test piece, the present embodiment are compared therewith using conventional dry blasting method.
Conventional dry blasting method substantially steps are as follows：
1）The test piece matrix surface for treating anodic oxidation carries out oil removing grease removal cleaning；
2）Dry blasting processing is carried out to test piece；
3）Supersonic flame spraying processing is carried out to test piece.
The concrete operation step of entire embodiment is as follows：
1）Matrix is the Ti6Al4V alloys disk totally 10 of 25 millimeters of diameter, 2 millimeters of thickness.
All 10 test pieces have carried out acetone ultrasonic cleaning first before roughening treatment, achieve the purpose that oil removing grease removal.
2）Dry blasting roughening treatment is carried out to wherein 5 test pieces.Dry spray is carried out to it using 220 mesh white alumina abrasive grains
Sand.Dry blasting compressed air pressure is 0.5 megapascal, and sandblasting distance is 300 millimeters, and sandblasting angle is 90 degree, and overlapping rate is 50%,
Sandblasting pass is 3 times.
Dry ice particles sandblasting roughening is carried out to other 5 test pieces.Dry ice is hexahedron dry ice particles, individual particle maximum ruler
Very little to be not less than 10 millimeters, per hour for 40 kilograms, dry ice spray gun to matrix distance is 25 millimeters to the flow of dry ice particles.
3）Supersonic flame thermal spraying treatment, spray parameters are carried out at the same time using specific tooling to above-mentioned all 10 test pieces
For spray gun TAFA5250, dusty spray Ni60,6.7 gallons of kerosene per hour, 1900 cubic feet per hour of oxygen, spraying away from
From 350 millimeters, 90 degree of spray angle.Thickness is about 40 microns.
Above-mentioned 2 kinds of test pieces are marked.It is C group test pieces that label, which lives through pretreated 5 test pieces of dry blasting,.Label
It is D group test pieces to live through 5 test pieces after dry ice particles injection.Above-mentioned two groups of test pieces all use supersonic speed fire in last step
The reason of flame spraying prepares one layer about 40 microns of coating be：The film layer of anodic oxidation is too thin, often nanoscale.Carry out
When metallographic observation, so thin film layer is very easy to obscure with inlay, it is not easy to distinguish the interface of film layer-matrix.Therefore, it adopts
With hot-spraying technique prepared by dry ice particles spray treatment and by dry blasting treated strip one layer it is about 40 micro-
The metal coating of rice, for protecting interface, convenient observation and analysis to interface.
Fig. 2 and Fig. 3 is the section metallograph using C groups and D groups respectively.Use ImageJ software assay surface pollution rates
（The ratio of total interface length shared by the exogenous impurity length of interface）, the interface pollution rate average value of each group sample is respectively：
A groups interface pollution rate is that 10.51%, B groups interface pollution rate is 3.05%.
As it can be seen that after the interface pollution of the matrix surface after dry ice particles spray treatment will be far superior to dry blasting processing
Matrix surface.
Both examples above proves, compared with conventional anodization pretreating process, using dry ice provided by the invention
Particle injection pretreating process can significantly reduce the interface pollution of film layer/basal body interface, while the combination for improving film layer is strong
Degree, biocompatibility and service life.
Claims (10)
1. preprocess method before a kind of Novel anode oxidation, which is characterized in that include the following steps：
1）Dry ice particles spray treatment is carried out to matrix surface；
1-1）Dry ice particles are handled, changes the size of dry ice particles or changes simultaneously the size and shape of dry ice particles；
Dry ice particles are processed as by cylinder, hexahedron or the octahedral bodily form using manufacture dry ice equipment, increase single dry ice particles
Cutting face；
1-2）Spray treatment is carried out to matrix surface；
Using spraying equipment, dry ice particles injection is carried out to matrix surface by suction-type spray regime or forced spray regime
Processing；Compressed air pressure ranging from 0.1~1.5 megapascal when injection；To the mesh for reaching purification, being roughened pretreating surface
's.
2. preprocess method before a kind of Novel anode oxidation according to claim 1, it is characterised in that：Step 1-1）Processing
The full-size of single dry ice particles size range, that is, individual particle afterwards is 5-15 millimeters, and dry ice range of flow is when injection
10-60 kilograms per hour.
3. preprocess method before a kind of Novel anode oxidation according to claim 2, it is characterised in that：Single dry ice particles
The full-size of size, that is, individual particle be not less than 10 millimeters, when injection dry ice flow be 40 kilograms per hour.
4. preprocess method before a kind of Novel anode oxidation according to claim 1, it is characterised in that：Step 1-2）In
Spray gun may be used in spraying equipment, and lance tube uses Lavalle mouth structure.
5. preprocess method before a kind of Novel anode oxidation according to claim 4, it is characterised in that：The nozzle of spray gun is straight
The distance range of ranging from 13-20 millimeters of diameter, spray gun to matrix is 15-50 millimeters.
6. preprocess method before a kind of Novel anode oxidation according to claim 1, it is characterised in that：It further include step 2）
To passing through step 1）Matrix surface after spray treatment carries out activation process；Workpiece table is activated using acid or alkaline activation liquid
Face achievees the purpose that activating surface.
7. preprocess method before a kind of Novel anode oxidation according to claim 6, it is characterised in that：Step 2）In work
Change liquid and selects single acid solution, or the alkaline solution using strong oxidizing property.
8. preprocess method before a kind of Novel anode oxidation according to claim 7, which is characterized in that acid solution uses
The mixture of nitric acid and hydrofluoric acid, ratio range are：100 milliliters of a concentration of 65-68% nitric acid：The hydrofluoric acid 5- of concentration >=40%
20 milliliters.
9. preprocess method before a kind of Novel anode oxidation according to claim 6, it is characterised in that：Step 2）In work
It is 10~30 seconds to change the time, ranging from 20~50 DEG C of tank liquor temperature.
10. preprocess method before a kind of Novel anode oxidation according to claim 9, it is characterised in that：Step 2）In
Soak time is combined as 15 seconds and 25 DEG C with tank liquor temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114108051A (en) * | 2021-12-24 | 2022-03-01 | 靖江先锋半导体科技有限公司 | Corrosion-resistant mixed acid anodic oxidation process |
| CN114144281A (en) * | 2019-06-07 | 2022-03-04 | 赛峰飞机发动机公司 | Blasting medium and surface treatment method using the same |
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