CN103866316A - Chemical passivation method of beryllium material - Google Patents
Chemical passivation method of beryllium material Download PDFInfo
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- CN103866316A CN103866316A CN201410067851.8A CN201410067851A CN103866316A CN 103866316 A CN103866316 A CN 103866316A CN 201410067851 A CN201410067851 A CN 201410067851A CN 103866316 A CN103866316 A CN 103866316A
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Abstract
The invention relates to a chemical passivation method of a beryllium material, belonging to the technical field of surface processing of the beryllium material. The chemical passivation method comprises the following steps: (1) wiping the surface of a machined beryllium material with an organic solvent; (2) drying the organic solvent on the surface of the beryllium material wiped by the organic solvent by using a blower; (3) carrying out ultrasonic cleaning on the beryllium material obtained in the step (2) by using an alcoholic solution; (4) carrying out chemical deoiling on the surface of the beryllium material; (5) carrying out weak etching on the surface of the beryllium material; (6) carrying out surface passivation on the beryllium material, namely immersing the beryllium material subjected to weak etching into a passivation solution, and carrying out passivation for 10-20 minutes at 35-45 DEG C. The chemical passivation processing method is simple in process composition, strong in operability and capable of being used for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of beryllium material chemical passivation treatment process, belong to beryllium material technical field of surface.
Background technology
Beryllium belongs to very unsettled metal on thermodynamics, exposes and can form one deck oxide film as thin as a wafer, the about 10nm of thickness of this layer of oxide film at ambient temperature.The oxide film of beryllium is generally made up of two-layer, and internal layer oxide film is the amorphous tight non-porous layer (also claiming blocking layer) near metallic surface, and the loose skin slightly thicker than internal layer.Internal layer oxide film is compressed in beryllium material surface, can form fine and close protective membrane, suppresses slightly corrosion, so under drying at room temperature atmospheric environment, the erosion resistance of beryllium material is fine.But beryllium is easily corroded in moist atmospheric environment, because its oxide film is thinner, do not have stronger antiseptic property.Now, the corrosion of beryllium material can be thought the extension of aqueous corrosion, and moisture or condensing water vapor in atmosphere provide electrolytic solution, causes beryllium and other impurity with oxide film local defect region to form miniature galvanic cell, there is galvanic corrosion, cause dissolving and the corrosion of metallic beryllium.Meanwhile, beryllium material is microalloy, the disperse Be that distributing on crystal boundary
2c precipitated phase (C content is conventionally 0.15%).Under wet gas environments, Be
2c precipitated phase meeting deferred reaction, is transformed into BeO and CH
4.Due to Be
2c is generally distributed on crystal boundary, Be
2c can be oxidized rapidly, makes beryllium material along grain boundary corrosion, thereby triggers the inefficacy mechanism of beryllium material.
Beryllium material is active metal-powder alloy material, and in atmosphere, its surface forms the very thin natural oxide film of one deck.Under drying at room temperature atmospheric environment, its erosion resistance is fine, but under moist atmosphere environment, corrosion resistance is poor.In order to meet the requirement of beryllium equipment structure part to Corrosion Protection, need to carry out surface treatment to beryllium equipment structure part.Beryllium material surface-treated object is: beryllium material, through rotproofing, makes its corrosion electrode potential in BeO passivation region, and generates the thicker BeO rete of one deck, stops the chemical corrosion of beryllium and the generation of galvanic corrosion.
Passivation Treatment is exactly to utilize the chemical reaction between metallic surface and chemical mediator solution to generate undissolved inorganic salt superficial film, to improve solidity to corrosion.Beryllium material chemical passivation processing is the most frequently used surface treatment process method, and can make beryllium material surface form one deck has the chemical passivation film of anti-corrosion function, improves its corrosion resistance nature.About the passivation of beryllium material, data from abroad introduction adopts concentrated nitric acid passivation, after passivation, on the surface of beryllium, form colourless beryllium oxide, its etch resistant properties can improve more than 4 times, but the rete consistence forming is poor, corrosion-resistant degree varies causes, in addition, passivating process adopts concentrated nitric acid operational danger large, and general cleaning is difficult to wash residual nitric acid in part blind hole, this will produce corrosive nature to part, and therefore product being adopted to nitric acid passivation is not best method.
Summary of the invention
The object of the invention is in order to overcome the deficiencies in the prior art, a kind of beryllium material chemical passivation treatment process is proposed, the method, for beryllium material part, meets the needs of product corrosion resistance nature, the method technique simple possible, workable, can be used for beryllium material chemical passivation processing.
The object of the invention is to be achieved through the following technical solutions.
A kind of beryllium material chemical passivation treatment process of the present invention, step is:
1) beryllium material surface organic solvent wiping: by the beryllium material piece surface organic solvent wiping after mechanical workout, it is conscientiously careful that wiping process needs, and each blind hole on part, threaded hole, groove inside also need careful wiping; The preferred acetone of organic solvent;
2) beryllium material surface blower dries up: the part that organic solvent wiping is completed, dry up remaining in surperficial organic solvent with blower, and the temperature that dries up process should be controlled at 35～45 ℃;
3) ethanolic soln ultrasonic cleaning: the beryllium material part after drying up is immersed in spirituous solution completely, then clean in supersonic cleaning machine, the frequency of supersonic cleaning machine is 30～40KHz, and the ultrasonic cleaning time is 10～20min, and the temperature of spirituous solution is 35～45 ℃.Spirituous solution is to be dissolved in 1000mL deionized water formulated by 800～1000mL dehydrated alcohol.
4) beryllium material surface chemistry oil removing: the beryllium material part after ultrasonic cleaning is immersed in sodium hydroxide solution, sodium hydroxide solution is to be dissolved in 1000mL deionized water formulatedly by 80～100g sodium hydroxide, keeps 25～35 ℃ of solution temperatures in electrochemical deoiling process.
5) the weak etch in beryllium material surface: carry out weak etch processing a little less than the beryllium material part that oil removing is completed immerses in etch solution, the etch time is 60～80s, the temperature of etch solution is 25～35 ℃, and weak etch solution is to be dissolved in the deionized water of 200～400mL formulated by the concentrated nitric acid of 600～800mL.
6) beryllium material surface passivating treatment: the beryllium material part that weak etch is completed is immersed in passivating dip, carries out Passivation Treatment.Passivating dip is the mixed solution of chromium trioxide, the Tripotassium iron hexacyanide, Sodium Fluoride and boric acid, be dissolved in the deionized water of 1000mL formulated by the Tripotassium iron hexacyanide, 3～5g Sodium Fluoride and the 1～2mL boric acid of the chromium trioxide of 5～8g, 2～5g, passivation time is 10～20min, and the temperature of passivation operation is 35～45 ℃.
Beneficial effect
Technique composition of the present invention is simple, workable, can be used for large-scale industrial production.
Electrochemical deoiling, the thoroughly stain such as greasy dirt, dust on cleaning components surface, makes the passive film surface uniform of generation continuous.Make in follow-up passivating process passivating dip can infiltrate uniformly the surface of part, improve the wetting property of piece surface and passivating dip, also strengthen the deoiling effect in part aperture and deep trouth simultaneously.
Weak etch processing, can remove the natural oxide film of piece surface, and affect hardly the roughness of piece surface, make beryllium matrix metal in the time of Passivation Treatment, can fully contact with chemical passivation solution, can improve the quality of beryllium piece surface passive film, be convenient to generate the passive film that bonding force is good, quality is high.
Beryllium material chemical passivation processing for the chemical property of beryllium material, adds a small amount of activator in the mixed solution of chromic acid and the Tripotassium iron hexacyanide, and in certain temperature range, metallic beryllium and chromic acid and the Tripotassium iron hexacyanide react, and generates BeOCr
2o
3, further forming the very thin inorganic salt rete of one deck on beryllium material surface, this membranous layer ingredient is comparatively complicated, and the main component of general rete is BeOxCr
2o
3yCrO
3zH
2o.
Accompanying drawing explanation
Fig. 1 is the 200 times of micrograms of beryllium material passivation test piece in example 1.
Embodiment
Embodiment 1
In sodium hydroxide solution, carry out electrochemical deoiling by being immersed in through the beryllium material test piece of ultrasonic cleaning, sodium hydroxide solution is to be dissolved in 1000mL deionized water formulated by 100g sodium hydroxide, in oil removing process, keep solution temperature between 25～30 ℃, carry out surface chemistry oil removing, oil removing time 5min; The beryllium material test piece that oil removing is completed is immersed in weak etch solution carries out weak etch processing, and the weak etch time is 60s, and the temperature of weak etch solution is 25 ℃, and weak etch solution is to be dissolved in the deionized water of 400mL formulated by the concentrated nitric acid of 600mL; The beryllium material part that activation is completed is immersed in passivating dip, carry out Passivation Treatment, passivating dip is dissolved in the deionized water of 1000mL formulated by the Tripotassium iron hexacyanide, 3g Sodium Fluoride and the commercially available boric acid of 2mL of the chromium trioxide of 8g, 5g, passivation time is 10min, and the temperature of passivation operation is between 35～45 ℃.
The beryllium material obtaining is tested as follows:
The outward appearance of passive film:
Beryllium material part is after chemical passivation is processed, and the surface of its passive film presents uniform iris to bronze-colored, and even film layer is continuous, surface compact, as shown in Figure 1.
Dimensional change before and after passivation:
Beryllium material is after chemical passivation is processed, and its dimensional change adopts milscale to measure, and dimensional change is-0.001～+ 0.001mm, and dimensional change is less, considers measuring error, can think that the size after Passivation Treatment does not change substantially.
Bonding strength:
The bonding strength of beryllium material chemical passivation film detects, and reference standard " QJ479-90 metal-plated coating bonding strength test method " adopts cross-hatching and thermal shock method to carry out.
Cross-hatching: adopt blade to draw the grid of 1mm × 1mm on the rete of part, peeling, obscission do not appear in rete at point of crossing place, and bonding strength is good.
Thermal shock method: part is heated to 220 ℃ and be incubated 30min, puts into immediately cold water after taking-up, chemical passivation rete has no peeling, obscission, and bonding strength is good.
Corrosion resistance nature:
The corrosion resistance nature of metal surface protection film detects, and conventionally adopts drop experiment.Drop experiment is to drip etchant solution on clean sample rete, occurs that using solution corrosion changes judgement and the appraisal standards of needed time as corrosion resisting property.The anti-corrosion test reference standard QJ471-88 of beryllium material passive film, selects 3% copper-bath to carry out spot test, records the time that test piece spot test reacts.Adopt the beryllium material part of passivation technology method provided by the invention processing, its solidity to corrosion improves 20 times than pure beryllium.
Embodiment 2
Change concentration of sodium hydroxide solution and oil removing time in electrochemical deoiling in embodiment 1,80g sodium hydroxide is dissolved in 1000mL deionized water formulated, in oil removing process, keeping solution temperature is 25～30 ℃, carries out surface chemistry oil removing, oil removing time 3min; All the other conditions are with embodiment 1.
The test piece of gained beryllium material, its passive film surface presents bronze-colored uniformly, and even film layer is continuous, surface compact, bonding force is good.
Embodiment 3
Change the weak etch time in embodiment 1, the etch time is 80s, and all the other conditions are with embodiment 1.
The test piece of gained beryllium material, its passive film surface presents bronze-colored uniformly, and even film layer is continuous, surface compact, bonding force is good.
Embodiment 4
Change weak etch strength of solution in embodiment 1, weak etch solution is to be dissolved in the deionized water of 200mL formulatedly by the concentrated nitric acid of 800mL, and all the other conditions are with embodiment 1.
The test piece of gained beryllium material, its passive film surface presents bronze-colored uniformly, and even film layer is continuous, surface compact, bonding force is good.
Embodiment 5
Change passivating dip concentration in embodiment 1, be dissolved in the deionized water of 1000mL formulatedly by the Tripotassium iron hexacyanide, 5g Sodium Fluoride and the 1mL boric acid of the chromium trioxide of 5g, 3g, all the other conditions are with embodiment 1.
The test piece of gained beryllium material, its passive film surface presents bronze-colored uniformly, and even film layer is continuous, surface compact, bonding force is good.
Embodiment 6
Change the Passivation Treatment time in embodiment 1, passivation time is 20min, and all the other conditions are with embodiment 5.
The test piece of gained beryllium material, its passive film surface presents bronze-colored uniformly, and even film layer is continuous, surface compact, bonding force is good.
The present invention not detailed description is known to the skilled person technology.
Claims (7)
1. a beryllium material chemical passivation treatment process, is characterized in that step is:
1) by the beryllium material surface machine solvent wiping after mechanical workout;
2) step 1) is dried up to its surperficial organic solvent with the beryllium material blower after organic solvent wiping;
3) by step 2) the beryllium material spirituous solution that obtains carries out ultrasonic cleaning;
4) beryllium material surface chemistry oil removing: the beryllium material part after ultrasonic cleaning is immersed in sodium hydroxide solution, keep 25～35 ℃ of solution temperatures in electrochemical deoiling process;
5) the weak etch in beryllium material surface: the beryllium material part that oil removing is completed immerses in weak etch solution and carries out weak etch processing, and the etch time is 60～80s, and the temperature of etch solution is 25～35 ℃;
6) beryllium material surface passivating treatment: the beryllium material part that weak etch is completed is immersed in passivating dip, carries out Passivation Treatment; Passivation time is 10～20min, and the temperature of passivation operation is 35～45 ℃.
2. a kind of beryllium material chemical passivation treatment process according to claim 1, is characterized in that: the organic solvent in step 1) is acetone.
3. a kind of beryllium material chemical passivation treatment process according to claim 1, is characterized in that: step 2) in dry up process temperature be 35～45 ℃.
4. a kind of beryllium material chemical passivation treatment process according to claim 1, it is characterized in that: in step 3), ultrasonic cleaning frequency is 30～40KHz, the ultrasonic cleaning time is 10～20min, the temperature of spirituous solution is 35～45 ℃, spirituous solution is the mixture of dehydrated alcohol and water, and the volume ratio of dehydrated alcohol and water is 8～10:10.
5. a kind of beryllium material chemical passivation treatment process according to claim 1, is characterized in that: in step 4), the concentration of sodium hydroxide solution is 80～100g/L.
6. a kind of beryllium material chemical passivation treatment process according to claim 1, is characterized in that: in step 5), in weak etch solution, the volume ratio of concentrated nitric acid and deionized water is 1.5-4:1.
7. a kind of beryllium material chemical passivation treatment process according to claim 1, it is characterized in that: in step 6), passivating dip is the mixed solution of chromium trioxide, the Tripotassium iron hexacyanide, Sodium Fluoride and boric acid, wherein by chromium trioxide: the Tripotassium iron hexacyanide: Sodium Fluoride: boric acid: deionized water=5～8g, 2～5g, 3～5g:1～2mL:1000mL.
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Cited By (3)
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| CN107236944A (en) * | 2017-06-19 | 2017-10-10 | 苏州莱特复合材料有限公司 | A kind of preparation method of auto parts powdered-metal passivator |
| CN112974798A (en) * | 2021-02-05 | 2021-06-18 | 哈尔滨工业大学 | Method for dustless treatment of beryllium powder |
| CN113764571A (en) * | 2021-09-07 | 2021-12-07 | 绍兴中芯集成电路制造股份有限公司 | Processing method of substrate with aluminum nitride film layer and preparation method of filter |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112974798A (en) * | 2021-02-05 | 2021-06-18 | 哈尔滨工业大学 | Method for dustless treatment of beryllium powder |
| CN113764571A (en) * | 2021-09-07 | 2021-12-07 | 绍兴中芯集成电路制造股份有限公司 | Processing method of substrate with aluminum nitride film layer and preparation method of filter |
| CN113764571B (en) * | 2021-09-07 | 2024-01-23 | 绍兴中芯集成电路制造股份有限公司 | Processing method of substrate with aluminum nitride film layer and preparation method of filter |
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