CN109186441A - The reagent of electroless nickel thickness, preparation method and application on coulomb method detection iron aluminium - Google Patents
The reagent of electroless nickel thickness, preparation method and application on coulomb method detection iron aluminium Download PDFInfo
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- CN109186441A CN109186441A CN201811126655.8A CN201811126655A CN109186441A CN 109186441 A CN109186441 A CN 109186441A CN 201811126655 A CN201811126655 A CN 201811126655A CN 109186441 A CN109186441 A CN 109186441A
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- reagent
- coulomb
- electroless nickel
- thickness
- iron aluminium
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/02—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
- G01B7/06—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness for measuring thickness
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- Measurement Of Length, Angles, Or The Like Using Electric Or Magnetic Means (AREA)
Abstract
The invention discloses the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium, phosphorus content is 6%~12% in the iron aluminium, and the reagent includes following components: chromic anhydride, boric acid.The reagent the preparation method comprises the following steps: under room temperature, 25~35g of chromic anhydride, 2~4g of boric acid are dissolved in 100mL water, mix, after completely dissolution, that is, be prepared into out coulomb method detection iron aluminium on electroless nickel thickness reagent.Using the reagent; using coulomb method electrolysis calibrator for detecting electroless nickel thickness on high ferrophosphorus aluminium, apparent potential change can be collected, shutdown obtains reliable thickness result; the reagent stability is high, can accurate detection go out electroless nickel thickness on high ferrophosphorus aluminium.
Description
Technical field
The present invention relates to technical field of chemical detection, more particularly to electroless nickel thickness on a kind of coulomb of method detection iron aluminium
Reagent, preparation method and application.
Background technique
Chemical nickel plating has very more advantages as novel environment friendly process for treating surface: the plating uniformity is very good, special
Not Shi He precision high workpiece through Overheating Treatment after plating can achieve very high hardness.In the prior art, common nickel plating
Thickness degree detection means has the detection of following three kinds: a, metallographic method；B, ray method detects；C, coulomb method, i.e. electrolysis thickness measuring.
Wherein, a, metallographic microscope method the disadvantage is that cut, are polished, micrometering, pretreatment its advantage is that precision is high
It takes a lot of time.B, ray detection, its advantage is that measuring speed is fast, 10 microns or less detection accuracy are high, the disadvantage is that at high cost.
C, it is electrolysed calibrator, i.e. coulomb method calibrator, its advantage is that detection speed is fast, measurement accuracy is high, the disadvantage is that point type plates damage layer,
But product sampling observation loss can be ignored.Currently used is coulomb method, i.e. electrolysis thickness measuring.
Currently on the market for low-phosphorous chemical nickel coulomb method thickness measuring agents useful for same, machine can detect measuring terminals,
And the case where for containing high phosphorus (phosphorus content is 6%~12%), because test process, without obvious potential change, machine acquires not
To measurement terminal, therefore accurate testing result is not reached.
Summary of the invention
In view of the above situation, the purpose of the present invention is to provide the examinations of electroless nickel thickness on a kind of coulomb of method detection iron aluminium
Agent, to solve the problems, such as that the prior art can not obtain accurate testing result for the chemical nickel plating of high content of phosphorus.
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, and phosphorus content is 6%~12% in the iron aluminium, institute
Stating reagent includes following components: chromic anhydride, boric acid.
Wherein, optionally, 25~35g of chromic anhydride, 2~4g of boric acid are contained in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 25g, boric acid 3g in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 35g, boric acid 3g in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 25g, boric acid 2g in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 35g, boric acid 4g in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 30g, boric acid 3g in reagent described in every 100mL.
As an alternative embodiment, containing chromic anhydride 28g, boric acid 3g in reagent described in every 100mL.
The present invention also provides the preparation methods of the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium, comprising:
Under room temperature, 25~35g of chromic anhydride, 2~4g of boric acid are dissolved in 100mL water, mixes, after completely dissolution, that is, is prepared into
Coulomb method detects the reagent of electroless nickel thickness on iron aluminium out.
The present invention also provides the applications of the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium, using coulomb method
It is electrolysed calibrator, the reagent that the above-mentioned coulomb method of institute detects electroless nickel thickness on iron aluminium is used for chemical nickel plating on high ferrophosphorus aluminium
Thickness, wherein the constant current of the coulomb method electrolysis calibrator is 7A/dm2, preset voltage 0.5V.
There is the prior art to compare, the present invention at least has the advantages that are as follows:
1, for chromic anhydride as oxidant, boric acid makees complexing agent, and the coating nickel ion of electrolysis is dissolved into chemical nickel test agent,
When the medium of electrolysis is all nickel-phosphorus alloy, with medium equipotential, and when electrolysis is to iron aluminium base, chromate and iron nickel aluminium
Cross reaction occurs for ion, and resistance generates variation, and current potential can be lifted quickly, and machine can collect apparent potential change, stop
Machine obtains reliable thickness as a result, therefore, for high phosphorus situation, can accurately detect the thickness for plating chemical nickel on tapping aluminium base.
2, reagent of the present invention meets GB/T4955-2005 electrolyte requirement: without in the case where impressed current not
It reacts with metal cladding；When coating by anodic solution to when penetrating and the matrix area exposed constantly increases, electrode
Detectable change dramatically should occur for current potential；
3, reagent cost of the present invention is low, and preparation method is simple, and operating method is easy when detection；It is effective to improve
The practicability of reagent of the present invention.
Detailed description of the invention
Above-mentioned and/or additional aspect of the invention and advantage will become from the description of the embodiment in conjunction with the following figures
Obviously and it is readily appreciated that, in which:
Fig. 1 is the potential diagram that embodiment 1 is tested；
Fig. 2 is the potential diagram that comparative example 1 is tested.
Specific embodiment
To keep objects, features and advantages of the present invention more obvious and easy to understand, with reference to the accompanying drawing to tool of the invention
Body embodiment is described in detail.Several embodiments of the invention are given in attached drawing.But the present invention can be with many not
With form realize, however it is not limited to embodiment described herein.On the contrary, purpose of providing these embodiments is makes to this
The disclosure of invention is more thorough and comprehensive.
Unless otherwise defined, all technical and scientific terms used herein and belong to technical field of the invention
The normally understood meaning of technical staff is identical.Term as used herein in the specification of the present invention is intended merely to description tool
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term " and or " used herein includes one or more phases
Any and all combinations of the listed item of pass.
Embodiments of the present invention propose the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium, solve existing
The problem of technology can not obtain accurate testing result for the chemical nickel plating of high content of phosphorus.
The reagent includes following components: chromic anhydride, boric acid.
Specifically, containing 25~35g of chromic anhydride, 2~4g of boric acid in reagent described in every 100mL.
The reagent the preparation method comprises the following steps:
Under room temperature, 25~35g of chromic anhydride, 2~4g of boric acid are dissolved in 100mL water, mixes, after completely dissolution, that is, is prepared into
Coulomb method detects the reagent of electroless nickel thickness on iron aluminium out.
Calibrator is electrolysed using coulomb method, the reagent that the above-mentioned coulomb method of institute detects electroless nickel thickness on iron aluminium is used for height
The thickness of chemical nickel plating on ferrophosphorus aluminium, wherein the constant current of the coulomb method electrolysis calibrator is 7A/dm2, preset voltage is
0.5V。
Divide multiple embodiments that the embodiment of the present invention is further detailed below.The embodiment of the present invention be not limited to
Under specific embodiment.Within the scope of the unchanged main rights, implementation can appropriate be changed.
Embodiment 1
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 25g in reagent described in every 100mL,
Boric acid 3g.
Under room temperature, chromic anhydride 25g, boric acid 3g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, potential diagram is as shown in Figure 1, from Fig. 1
As it can be seen that 5 equipotentials of electroless nickel layer tie-in, reagent strong antijamming capability, terminal identification is accurate, and final thickness detects average result
Are as follows: 5.314 μm.
This is because for chromic anhydride as oxidant, boric acid makees complexing agent, and the coating nickel ion of electrolysis is dissolved into chemistry in reagent
In nickel test agent.When the medium of electrolysis is all nickel-phosphorus alloy, with medium equipotential.When electrolysis to arrive iron aluminium base when, chromium
Cross reaction occurs for acid group and iron nickel aluminium ion, and resistance generates variation, and current potential can be lifted quickly, and machine is enabled to collect electricity
Position variation, which is shut down, obtains reliable thickness result.
In addition, this test agent meets GB/T4955-2005 electrolyte requirement: 1, without in the case where impressed current not with
Metal cladding reacts；2, when coating by anodic solution to when penetrating and the matrix area exposed constantly increases, electrode
Detectable change dramatically should occur for current potential.
The reagent cost is low, and preparation method is simple, and operating method is easy when detection；It effectively raises of the present invention
The utilization rate of reagent.
Embodiment 2
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 35g in reagent described in every 100mL,
Boric acid 3g.
Under room temperature, chromic anhydride 35g, boric acid 3g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, final thickness detects average result
Are as follows: 5.308 μm.
Embodiment 3
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 25g in reagent described in every 100mL,
Boric acid 2g.
Under room temperature, chromic anhydride 25g, boric acid 2g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, final thickness detects average result
Are as follows: 5.311 μm.
Embodiment 4
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 35g in reagent described in every 100mL,
Boric acid 4g.
Under room temperature, chromic anhydride 35g, boric acid 4g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, final thickness detects average result
Are as follows: 5.316 μm.
Embodiment 5
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 30g in reagent described in every 100mL,
Boric acid 3g.
Under room temperature, chromic anhydride 30g, boric acid 3g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, final thickness detects average result
Are as follows: 5.309 μm.
Embodiment 6
A kind of coulomb of method detects the reagent of electroless nickel thickness on iron aluminium, contains chromic anhydride 28g in reagent described in every 100mL,
Boric acid 3g.
Under room temperature, chromic anhydride 28g, boric acid 3g are dissolved in 100mL water, sufficiently dissolution, mixing；It is prepared into out the detection of coulomb method
The reagent of electroless nickel thickness on iron aluminium.
Reagent described in the present embodiment is identical as the application method of available reagent.
The chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of 5.3 μm, the uniformity is ± 5%, is surveyed
Thick instrument provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5 times, final thickness detects average result
Are as follows: 5.318 μm.
Comparative example 1
Using national standard iron nickel plating reagent A 5, the chemical nickel standard film that KOCOUR phosphorus content in the U.S. is 12% is tested, with a thickness of
5.3 μm, the uniformity is ± 5%, and calibrator provides constant current 7A/dm2, preset voltage 0.5V electro deposition, follow-on test 5
Secondary, final thickness detects average result are as follows: 5.318 μm.Twice, potential diagram is as shown in Fig. 2, as it is clear from fig. 2 that curve for follow-on test
Current potential disorder, surface oxide layer current potential is high, is then lowered into chemical nickel thickness potential duration and raises up, terminal current potential and take-off potential
In a potential levels, whether the accurate judgement that machine is difficult arrives substrate and makes reliable test result, therefore can not detect thickness.
Following table compared the testing result of above-mentioned each embodiment and two comparative examples:
| Standard thickness (μm) | It detects thickness (μm) | |
| Embodiment 1 | 5.3 ± 5% | 5.314 |
| Embodiment 2 | 5.3 ± 5% | 5.308 |
| Embodiment 3 | 5.3 ± 5% | 5.311 |
| Embodiment 4 | 5.3 ± 5% | 5.316 |
| Embodiment 5 | 5.3 ± 5% | 5.309 |
| Embodiment 6 | 5.3 ± 5% | 5.318 |
| Comparative example 1 | 5.3 ± 5% | It can not detect thickness |
As can be seen from the above table, it is capable of detecting when to plate chemical nickel on high ferrophosphorus aluminium using the reagent of various embodiments of the present invention
Thickness, and testing result precision is higher, and can not detect to plate chemical nickel on high ferrophosphorus aluminium using national standard iron nickel plating reagent A 5
Thickness.
In conclusion the prior art is compared, the present invention is at least had the advantages that are as follows:
1, for chromic anhydride as oxidant, boric acid makees complexing agent, and the coating nickel ion of electrolysis is dissolved into chemical nickel test agent,
When the medium of electrolysis is all nickel-phosphorus alloy, with medium equipotential, and when electrolysis is to iron aluminium base, chromate and iron nickel aluminium
Cross reaction occurs for ion, and resistance generates variation, and current potential can be lifted quickly, and machine can collect apparent potential change, stop
Machine obtains reliable thickness as a result, therefore, for high phosphorus situation, can accurately detect the thickness for plating chemical nickel on tapping aluminium base.
2, reagent of the present invention meets GB/T4955-2005 electrolyte requirement: without in the case where impressed current not
It reacts with metal cladding；When coating by anodic solution to when penetrating and the matrix area exposed constantly increases, electrode
Detectable change dramatically should occur for current potential；
3, reagent cost of the present invention is low, and preparation method is simple, and operating method is easy when detection；It is effective to improve
The practicability of reagent of the present invention.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium, which is characterized in that phosphorus content is 6% in the iron aluminium
~12%, the reagent includes following components: chromic anhydride, boric acid.
2. the reagent of electroless nickel thickness on according to claim 1 coulomb of method detection iron aluminium, which is characterized in that every
Contain 25~35g of chromic anhydride, 2~4g of boric acid in reagent described in 100mL.
3. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 25g, boric acid 3g in reagent described in 100mL.
4. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 35g, boric acid 3g in reagent described in 100mL.
5. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 25g, boric acid 2g in reagent described in 100mL.
6. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 35g, boric acid 4g in reagent described in 100mL.
7. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 30g, boric acid 3g in reagent described in 100mL.
8. the reagent of electroless nickel thickness on according to claim 2 coulomb of method detection iron aluminium, which is characterized in that every
Contain chromic anhydride 28g, boric acid 3g in reagent described in 100mL.
9. the preparation method of the reagent of electroless nickel thickness on a kind of coulomb of method detection iron aluminium characterized by comprising
Under room temperature, 25~35g of chromic anhydride, 2~4g of boric acid are dissolved in 100mL water, mixes, after completely dissolution, that is, is prepared into outbound
Human relations method detects the reagent of electroless nickel thickness on iron aluminium.
10. the application of the reagent of electroless nickel thickness on described in claim 1 coulomb of method detection iron aluminium, which is characterized in that adopt
It is electrolysed calibrator with coulomb method, the reagent that the coulomb method detects electroless nickel thickness on iron aluminium is used on high ferrophosphorus aluminium chemical
The thickness of nickel plating, wherein the constant current of the coulomb method electrolysis calibrator is 7A/dm2, preset voltage 0.5V.
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| CN201811126655.8A CN109186441A (en) | 2018-09-26 | 2018-09-26 | The reagent of electroless nickel thickness, preparation method and application on coulomb method detection iron aluminium |
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| SU1763874A1 (en) * | 1990-07-16 | 1992-09-23 | Институт химии твердого тела и переработки минерального сырья СО АН СССР | Method of coulometric measurements of metal cover thickness of objects |
| CN101109093A (en) * | 2007-07-16 | 2008-01-23 | 中南大学 | Method for electrodepositing nanocrystalline chromium-nickel alloy coating with carboxylic acid or its salt -urea impulse |
| CN106705826A (en) * | 2017-03-15 | 2017-05-24 | 四维尔丸井(广州)汽车零部件有限公司 | Test method for plating thickness of electroplated part |
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2018
- 2018-09-26 CN CN201811126655.8A patent/CN109186441A/en active Pending
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| SU1650796A1 (en) * | 1988-08-24 | 1991-05-23 | Предприятие П/Я А-3771 | Coulometric method for determination of coat thickness |
| SU1679349A1 (en) * | 1989-01-12 | 1991-09-23 | Институт Химии И Химической Технологии Ан Литсср | Solution for coulometric determination of chromic coating thickness |
| SU1763874A1 (en) * | 1990-07-16 | 1992-09-23 | Институт химии твердого тела и переработки минерального сырья СО АН СССР | Method of coulometric measurements of metal cover thickness of objects |
| CN101109093A (en) * | 2007-07-16 | 2008-01-23 | 中南大学 | Method for electrodepositing nanocrystalline chromium-nickel alloy coating with carboxylic acid or its salt -urea impulse |
| CN106705826A (en) * | 2017-03-15 | 2017-05-24 | 四维尔丸井(广州)汽车零部件有限公司 | Test method for plating thickness of electroplated part |
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