CN102051610A - Beryllium part passivating process - Google Patents
Beryllium part passivating process Download PDFInfo
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- CN102051610A CN102051610A CN 201010620182 CN201010620182A CN102051610A CN 102051610 A CN102051610 A CN 102051610A CN 201010620182 CN201010620182 CN 201010620182 CN 201010620182 A CN201010620182 A CN 201010620182A CN 102051610 A CN102051610 A CN 102051610A
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Abstract
The invention relates to a beryllium part passivating process comprising the following steps: 1, deoiling by an ultrasonic alcohol medium; 2, carrying out acid dipping treatment on the deoiled beryllium part; and 3, passivating. In the invention, the pretreatment procedure of the part is strengthened, and the chemical deoiling and acid dipping procedures are added, thus solving the problem of the wetting property of the part surface with a solution, and simultaneously improving the deoiling effect on small holes and deep grooves of the part; the formula and parameters of the acid dipping solution are determined by a large number of experiments, and the acid dipping solution can remove a natural passivating film but has a slight influence on the roughness of the part surface; and by removing the natural passivating film by a chemical method, the quality of the beryllium passivating film layer is improved, and a passivating film with good binding force and high quality can be generated.
Description
Technical field
The present invention relates to a kind of beryllium part passivation technology.
Background technology
Metallic beryllium is the lightest alkaline-earth metal, have density little (be aluminium 2/3), modulus of elasticity height (be aluminium 5 times), than stiffness height (be aluminium 6.4 times), thermal expansivity is little, dimensional stability good, can keep the original characteristics such as size of product in hundreds of degree scopes.Metallic beryllium has become the excellent material of aircraft and guided missile structure spare.Both at home and abroad gyro in the space flight high precision type product, the primary structure part that adds platforms such as table, stage body all adopt beryllium material (RJY-40), and gyro, the part that adds table all need certain corrosion-resistanting decoration performance.External beryllium material part adopts passivation technology to satisfy the needs of product performance mostly, and the beryllium passivation technology is seldom on the books in the data document at home.Adopt the organic oil removing of gasoline before in the past piece surface being handled during oil removing, cause the piece surface oil removing not thorough, therefore the film surface quality is inhomogeneous continuously after the passivation, and Passivation Treatment utilizes the non-electrolytics reaction between metallic surface and solution to produce undissolved inorganic salt superficial film, to improve solidity to corrosion.Passivation about the beryllium material, the concentrated nitric acid passivation is adopted in the pertinent data introduction, form colourless beryllium oxide after the passivation on the surface of beryllium, this rete can improve etch resistant properties more than 4 times, but the rete consistence that forms is poor, corrosion-resistant degree varies causes, in addition, passivating process adopts the concentrated nitric acid operational danger big, and general cleaning is difficult to wash residual nitric acid in the part blind hole, this will produce corrosive nature to part, and therefore product being adopted the nitric acid passivation is not best method.Therefore the subject matter that exists of prior art is anticorrosion poor performance after the passivation of beryllium part, influences the use properties and the life-span of beryllium part.
Summary of the invention
In order to solve the problem of beryllium part antiseptic property difference in the prior art, the invention provides a kind of beryllium part passivation technology.
Technical scheme of the present invention is: a kind of beryllium part passivation technology comprises following performing step:
Step 1: adopt ultrasonic wave alcohol medium to carry out oil removal treatment;
Step 2: the beryllium part after the oil removal treatment is carried out weak etch handle;
Step 3: Passivation Treatment.
Preceding electrochemical deoiling treatment step was handled in weak etch after method of the present invention also comprised ultrasonic wave alcohol medium oil removal treatment; Described electrochemical deoiling is handled and is adopted Na
2CO
310H
2O concentration is that 40～50g/L, NaOH concentration are 3～5g/L and Na
3PO
4Concentration be the degreasing fluid of 20～30g/L, be 3～5min in the oil removing time, remove oil temperature and be under 60～80 ℃ the condition and carry out.
Method of the present invention also comprises the beryllium part sealing treatment step after the Passivation Treatment; Described sealing treatment is to adopt deionized water to wash under 95～100 ℃ condition.
It is to be 15～38 ℃ in the etch temperature that above-mentioned weak etch is handled, and the etch time is to carry out under the condition of 15～20s; HNO in the etch solution that described weak etch is handled
3Concentration is 25mL/L, ρ=1.63, and deionized water concentration is 75mL/L.
Above-mentioned Passivation Treatment adopts Na
2Cr
2O
7Concentration is that 3～3.5g/L, activator concentration are the passivating dip of 0.8～1g/L, is 45～50 ℃ at passivation temperature, carries out under the condition of passivation time for 3min at least.
Beryllium part passivation technology of the present invention has the following advantages:
1, the present invention strengthens the pretreatment procedure to part, increases electrochemical deoiling and weak etch operation, has solved the wetting property of piece surface and solution, has improved simultaneously deoiling effect in part aperture and the deep trouth.
2, the present invention has determined the prescription and the parameter of weak etch solution by a large amount of experiments, can remove the nature passive film by weak etch solution, but the roughness influence to piece surface is very little, utilize chemical process to remove the nature passive film, improve the quality of beryllium passivation film, be convenient to generate the passive film that bonding force is good, quality is high.
3, passivating solution of the present invention adds a spot of activator in the mixed solution of chromic acid and dichromate, and in certain temperature range, metallic beryllium and chromic acid and dichromate react, and generates Cr
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 x Cr
2O
3Y CrO
3ZH
2O, and contain very micro-beryllium ion, this rete can improve the etch resistant properties of part more than 5 times.This formulation cost is cheap, and is simple to operate.
4, the present invention seals under 95～100 ℃ the condition in deionized water through the beryllium part after the passivation, passive film will generate hydration passivation beryllium in the process of sealing, to reach the effect of sealing of hole, prevent and in the follow-up process of depositing and processing, adsorb obnoxious flavour, impurity and airborne moisture, cause the passivation film visual appearance poor, the phenomenon that corrosion resistance descends rapidly.
5, determined the passivation technology of beryllium part by a large amount of experiments, this technological operation is simple, with low cost, can improve the corrosion resistance of part, and has certain decorate properties, and this process stabilizing is reliable.
Embodiment
A kind of beryllium part passivation technology involved in the present invention, its preferred implementation is:
This processing method comprises following performing step:
Step 1: adopt ultrasonic wave alcohol medium to carry out organic oil removal treatment; Usually after adopting the gasoline oil removing in the existing method, because gasoline and water mutual solubility are bad, often passivating dip can not soak into the surface of part uniformly in follow-up passivating process, therefore the present invention changes the organic oil removing of gasoline the oil removing of into ultrasonic alcohol medium, so not only solved the wetting property of piece surface and solution, improved simultaneously deoiling effect in part aperture and the deep trouth.
Step a: electrochemical deoiling is handled; Adopt chemicals to carry out the chemical process oil removing again through after in ultrasonic wave alcohol medium, carrying out organic oil removing, in order further to improve the deoiling effect of part, according to the chemical property of beryllium metal and the prescription of metalloid electrochemical deoiling in the past, prescription and parameter to electrochemical deoiling have been carried out further optimization, and promptly electrochemical deoiling is handled in the degreasing fluid that is adopted and contained Na
2CO
310H
2O concentration is that 40～50g/L, NaOH concentration are 3～5g/L and Na
3PO
4Concentration be 20～30g/L, be 3～5min in the oil removing time, remove oil temperature and be under 60～80 ℃ the condition and carry out, referring to table 1.
Table 1 electrochemical deoiling prescription and parameter
| Na 2CO 3·10H 2O | 40～50g/L |
| NaOH | 3～5g/L |
| Na 3PO 4 | 20～30g/L |
| Remove oil temperature | 60～80℃ |
| The oil removing time | 3～5min |
Step 2: the beryllium part before the oil removal treatment post-passivation is carried out weak etch handle.Beryllium part after organic oil removing and/or the processing of electrochemical deoiling method embathes through in the weak etch solution again, carries out weak etch and handles.
Because beryllium is more active metal, in air, be easy to form natural oxide film as thin as a wafer, this oxide film does not possess corrosion resistance, but undesirable action is played in the growth to follow-up passive film, in order to improve the quality of beryllium passivation film, be convenient to generate the passive film that bonding force is good, quality is high, the present invention adopts weak etch to handle.
HNO in the weak etch solution that is adopted is handled in weak etch of the present invention
3Concentration is that 25mL/L, ρ=1.63, deionized water concentration are 75mL/L, and is 15～38 ℃ in the etch temperature, and the etch time is to carry out under the condition of 15～20s, promptly referring to table 2.
The prescription and the parameter of the weak etch solution of table 2
| HNO 3 | ρ＝1.63 | 25mL/L |
| Deionized water | 75mL/L | |
| The etch temperature | 15～38℃ | |
| The etch time | 15～20s |
Step 3: the part after the oil removing is carried out Passivation Treatment.
Beryllium part after oil removing, weak etch are handled can carry out Passivation Treatment, and Passivation Treatment is exactly the beryllium part after the pre-treatment to be put into contain the Na that concentration is 3～3.5g/L
2Cr
2O
7And concentration is to carry out passivation in the passivating dip of activator of 0.8～1/L, and passivation temperature is controlled in 45～50 ℃ of scopes, and passivation time generally is controlled in 3～5 scopes, but when handling big part the proper extension passivation time, referring to table 3.
Table 3 is the prescription and the parameter of passivating dip
| Na 2Cr 2O 7 | 3～3.5g/L |
| Activator | 0.8～1g/L |
| Service temperature | 45～50℃ |
| Passivation time | More than the 3min |
For the active metal passivation, often adopt the passivating method of chromic acid or dichromate in the process of surface treatment, the rete that produces by this method generally is different colors, mostly be iris, at the chemical property of beryllium material, its passivation principle is: add a spot of activator in the mixed solution of chromic acid and dichromate, in certain temperature range, metallic beryllium and chromic acid and dichromate react, and generate Cr
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 xCr
2O
3Y CrO
3Z H
2O, and contain very micro-beryllium ion, this rete can improve the etch resistant properties of part more than 5 times, and this formulation cost is cheap, and is simple to operate.
Step 4: the beryllium part after passivation carries out the deionization washing.
Because the beryllium material belongs to powder metallurgy mostly, after passivation, passivation film has certain porosity, in the follow-up process of depositing and processing, adsorb obnoxious flavour, impurity and airborne moisture easily, cause the passivation film visual appearance poor, corrosion resistance descends rapidly, in conjunction with the characteristics of passive film, the present invention washes in deionized water through the beryllium part after the Passivation Treatment again, to reach the effect of sealing of hole.
The beryllium part that passivation technology of the present invention is produced is tested its passive film performance, and test result is:
1, rete outward appearance: the passivation film that carries out of adopting new technology is that uniform iris is extremely bronze-colored, and rete is continuous, does not have other mass defect.
2, corrosion resistance nature: 5% CuSO is adopted in the inspection of corrosion resistance nature
4Spot test, test-results sees Table 4.
Table 4: corrosion resistant test contrast table
| Sample type | Main salt | The passivation mode | The beginning reaction times | Rete reddens the time |
| Pure beryllium | 30s | 45s | ||
| The beryllium passive film | CrO 3、K 2Cr 2O 7 | 3～5min | 1～2min | 5～8min |
The beryllium passivating film characteristics that beryllium part passivating process of the present invention produces:
1, the test specimen after beryllium part passivating process of the present invention passivation, size reduction 0～2 μ m of test specimen, Film color are that iris is to bronze-colored.
2, the rete corrosion resistance improves more than 5 times than pure beryllium.
Claims (7)
1. beryllium part passivation technology is characterized in that: may further comprise the steps:
1] adopt ultrasonic wave alcohol medium to carry out oil removal treatment;
2] the beryllium part after the oil removal treatment being carried out weak etch handles;
3] Passivation Treatment.
2. beryllium part passivation technology according to claim 1 is characterized in that: preceding electrochemical deoiling treatment step is handled in weak etch after also comprising ultrasonic wave alcohol medium oil removal treatment; Described electrochemical deoiling is handled and is adopted Na
2CO
310H
2O concentration is that 40～50g/L, NaOH concentration are 3～5g/L and Na
3PO
4Concentration be the degreasing fluid of 20～30g/L, be 3～5min in the oil removing time, remove oil temperature and be under 60～80 ℃ the condition and carry out.
3. beryllium part passivation technology according to claim 1 and 2 is characterized in that: also comprise the beryllium part sealing treatment step after the Passivation Treatment; Described sealing treatment is to adopt deionized water to wash under 95～100 ℃ condition.
4. beryllium part passivation technology according to claim 3 is characterized in that: it is to be 15～38 ℃ in the etch temperature that described weak etch is handled, and the etch time is to carry out under the condition of 15～20s; HNO in the etch solution that described weak etch is handled
3Concentration is 25mL/L, ρ=1.63, and deionized water concentration is 75mL/L.
5. beryllium part passivation technology according to claim 3 is characterized in that: described Passivation Treatment adopts Na
2Cr
2O
7Concentration is that 3～3.5g/L, activator concentration are the passivating dip of 0.8～1g/L, is 45～50 ℃ at passivation temperature, carries out under the condition of passivation time for 3min at least.
6. beryllium part passivation technology according to claim 1 and 2 is characterized in that: it is to be 15～38 ℃ in the etch temperature that described weak etch is handled, and the etch time is to carry out under the condition of 15～20s; HNO in the etch solution that described weak etch is handled
3Concentration is 25mL/L, ρ=1.63, and deionized water concentration is 75mL/L.
7. beryllium part passivation technology according to claim 1 and 2 is characterized in that: described Passivation Treatment adopts Na
2Cr
2O
7Concentration is that 3～3.5g/L, activator concentration are the passivating dip of 0.8～1g/L, is 45～50 ℃ at passivation temperature, carries out under the condition of passivation time for 3min at least.
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|---|---|---|---|
| CN 201010620182 CN102051610A (en) | 2010-12-31 | 2010-12-31 | Beryllium part passivating process |
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|---|---|---|---|
| CN 201010620182 CN102051610A (en) | 2010-12-31 | 2010-12-31 | Beryllium part passivating process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866298A (en) * | 2014-02-27 | 2014-06-18 | 北京航天控制仪器研究所 | Chemical nickel-plating pretreatment method for beryllium product |
| CN103866316A (en) * | 2014-02-27 | 2014-06-18 | 北京航天控制仪器研究所 | Chemical passivation method of beryllium material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392283A (en) * | 2002-07-09 | 2003-01-22 | 华中科技大学 | Hot dipping aluminium and aluminium alloy inactivation process of plating |
-
2010
- 2010-12-31 CN CN 201010620182 patent/CN102051610A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1392283A (en) * | 2002-07-09 | 2003-01-22 | 华中科技大学 | Hot dipping aluminium and aluminium alloy inactivation process of plating |
Non-Patent Citations (2)
| Title |
|---|
| 《粘接技术手册》 20010831 张玉龙等 铍及铍合金 中国轻工业出版社 180-181 1-7 , 第1版 1 * |
| 《航天工艺》 19900831 孙其玉 《铍陀螺零件的阳极氧化工艺》 22-24，26 2-3 , 第4期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103866298A (en) * | 2014-02-27 | 2014-06-18 | 北京航天控制仪器研究所 | Chemical nickel-plating pretreatment method for beryllium product |
| CN103866316A (en) * | 2014-02-27 | 2014-06-18 | 北京航天控制仪器研究所 | Chemical passivation method of beryllium material |
| CN103866298B (en) * | 2014-02-27 | 2016-03-02 | 北京航天控制仪器研究所 | A kind of beryllium material chemical nickel plating pre-treating process |
| CN103866316B (en) * | 2014-02-27 | 2016-05-04 | 北京航天控制仪器研究所 | A kind of beryllium material chemical passivation processing method |
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Application publication date: 20110511 |