CN102277587A - Method for removing hard multi-component nitride reaction film - Google Patents
Method for removing hard multi-component nitride reaction film Download PDFInfo
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- CN102277587A CN102277587A CN2011102148226A CN201110214822A CN102277587A CN 102277587 A CN102277587 A CN 102277587A CN 2011102148226 A CN2011102148226 A CN 2011102148226A CN 201110214822 A CN201110214822 A CN 201110214822A CN 102277587 A CN102277587 A CN 102277587A
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Abstract
The invention relates to a method for removing a hard multi-component nitride reaction film, which comprises the following steps of: determining sodium gluconate, sodium hydroxide, hydrogen peroxide containing 30% H2O2, sodium dodecyl sulfate, sodium tripolyphosphate and distilled water as raw materials to prepare a removing liquid; preparing the removing liquid; and determining the removing technology. The method is simple and convenient to operate, and coating film layers on the surfaces of various shapes of workpieces can be completely removed.
Description
Technical field
The present invention relates to a kind of stripping method of nitride film, particularly adopt the stripping method of the multicomponent nitride hard reaction film of vacuum coating technology preparation.
Background technology
Vacuum coating technology is widely used in the preparation process of various hard reaction films, has played good modifying function for the surface strengthening of cutter, mould and other wearing pieces.Early stage hard reaction film mainly is titanium nitride (TiN), develops into TiAlN (TiAlN), titanium nitride zirconium (TiZrN) and TiAlN zirconium multicomponent nitride hard reaction films such as (TiAlZrN) gradually.Yet, owing to the surface treatment of plating piece, many-sided reasons such as control of vacuum plating process, the time regular meeting the not good situation of coating quality appears, such as, hardness is not high enough, sticking power is strong, rete local shedding etc.In case such situation takes place, these plating pieces just can not directly carry out plated film again, otherwise that coating quality will become will be poorer.For this reason, the workpiece that these need to not plated carries out surface treatment, strips original superficial film, obtains the more surface of the work of cleaning.This just requires 2 points, and the first, original coatings stripping is clean; The second, it is smooth and do not have evidence of corrosion, do not have the machinery scratch to keep moving back workpiece surface behind the film.
At present, the main method of stripping poor quality's rete is: 1, mechanical polishing, this method is only applicable to the workpiece that surface shape is simple, be easy to grinding and polishing, for shape a little complex surfaces then be difficult to carry out, in addition, in polishing process, the situation that rete is difficult to strip fully or scratch workpiece surface appears easily; 2, chemistry stripping mainly is to use aqueous hydrogen peroxide solution that film-coating workpiece is soaked, and the general time is longer, and is not easy stripping.
Summary of the invention
The stripping method that the purpose of this invention is to provide a kind of multicomponent nitride hard reaction film, this stripping method is easy and simple to handle, the coatings of different shape workpiece surface can be stripped fully.
Technical scheme of the present invention is: a kind of stripping method of multicomponent nitride hard reaction film is;
1, determining of stripping liquid raw material: determine gluconic acid sodium salt, NaOH, contain 30%H
2O
2Hydrogen peroxide, dodecyl sodium sulfate, sodium phosphate trimer, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step adds mass percent in the glass container and is 63.5% ~ 68% distilled water; Second step adds mass percent in the glass container and is 1.5% ~ 3.5% gluconic acid sodium salt, stirs until fully dissolving; The 3rd step slowly added mass percent in the glass container and is 6.5% ~ 10% NaOH, put the medicine rapid stirring on one side until whole the dissolving in course of dissolution, can discharge a certain amount of heat, caused that temperature slightly rises; The 4th step, be that 0.2% ~ 0.4% dodecyl sodium sulfate powder and mass percent are that 0.2% ~ 0.4% sodium phosphate trimer powder is composite with mass percent, wherein, the ratio of the mass fraction of dodecyl sodium sulfate and sodium phosphate trimer is between the 1:1 to 1:0.7, and the mass percent sum of the two must be in 0.4% ~ 0.8%, mixes then, pour in the glass container, and the quick manual stirring, stop after 8 ~ 10 minutes stirring, naturally cool to room temperature; In the 5th step, add mass percent in the glass container and be 20% ~ 25% the 30%H that contains
2O
2Hydrogen peroxide, wherein, NaOH with contain 30%H
2O
2The ratio of mass fraction of hydrogen peroxide be between the 1:3.5 to 1:2, and the mass percent sum of the two must be between 29% ~ 33%, stirs then, obtains stripping liquid.
3, determining of stripping technology: for sake of convenience, the sample of following plating multicomponent nitride hard reaction film abbreviates the plated film sample as, the first step, the plated film sample is connected with anchor and fixing with Stainless Steel Wire, wherein anchor places the Glass Containers top, and the plated film sample places above-mentioned stripping liquid, keeps vertically, guarantee that simultaneously the plated film sample is soaked in the stripping liquid, does not contact with Glass Containers bottom and sidewall; In second step, the colour-change of the sample surfaces that detects by an unaided eye can find that color shoals gradually, metallic matrix color and metalluster before becoming plated film not; In the 3rd step, the plated film sample move back behind the film is taken out in the rete of the sample surfaces to be coated back that reacts completely, that is, stripping TiAlN film and TiAlZrN film time are 30 minutes; The stripping TiZrN film time is 120 minutes; In the 4th step, move back plated film sample surfaces 2 minutes behind the film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample behind the film after 1 minute and dry up.
Stripping method according to multicomponent nitride hard reaction film proposed by the invention, can strip the multicomponent nitride hard reaction film of plating on the metallic matrix fully, thicknesses of layers is approximately 1.5 microns ~ 2 microns, move back the plated film sample surfaces light behind the film, has metalluster, and the employing energy spectrum analysis, the plated film sample surfaces composition that moves back behind the film is consistent with uncoated metallic matrix, detects less than titanium (Ti), aluminium (Al), zirconium (Zr), nitrogen (N) element; The stripping technology that the present invention proposes is simple and clear, easy handling; Determine the mass percent scope of a moiety in the stripping liquid and the qualified relation between each moiety, guaranteed to move back the repeatability of film effect.
Embodiment
Below in conjunction with embodiment the present invention is described in further detail.
Embodiment 1
The stripping method of the titanium aln precipitation hard reaction film of plating on the stainless steel base
1, determining of stripping liquid raw material: determine gluconic acid sodium salt, NaOH, contain 30%H
2O
2Hydrogen peroxide, dodecyl sodium sulfate, sodium phosphate trimer, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step adds mass percent in the glass container and is 200 milliliters of 68% distilled water; Second step adds mass percent in the glass container and is 2% gluconic acid sodium salt 6 grams, stirs until fully dissolving; The 3rd step slowly added mass percent in the glass container and is 8.5% NaOH 25 grams, put the medicine rapid stirring on one side until whole the dissolving in course of dissolution, can discharge a certain amount of heat, caused that temperature slightly rises; The 4th step, be 0.3% dodecyl sodium sulfate (powder), 1 gram with mass percent with mass percent be that 0.2% sodium phosphate trimer (powder) 0.6 gram is composite, wherein, dodecyl sodium sulfate is 1:0.7 with the ratio of the mass fraction of sodium phosphate trimer, and the mass percent sum of the two is 0.5%, mixes, pour in the glass container, and the quick manual stirring, stop after 8 ~ 10 minutes stirring, naturally cool to room temperature; In the 5th step, add mass percent in the glass container and be 21% the 30%H that contains
2O
255 milliliters in hydrogen peroxide, wherein, NaOH with contain 30%H
2O
2The ratio of mass fraction of hydrogen peroxide be 1:2.5, and the mass percent sum of the two is 29.5%, stirs then, obtains stripping liquid.
3, determining of stripping technology: the first step, (thicknesses of layers is about 1.5 microns with plating titanium aln precipitation (TiAlN) hard reaction film on the stainless steel base with Stainless Steel Wire, titanium, aluminium, the plated film sample (being of a size of 40 millimeters * 30 millimeters * 1 millimeter) that the nitrogen-atoms ratio is approximately Ti:Al:N=0.35:0.2:0.45) is connected with anchor and is fixing, wherein anchor places the Glass Containers top, the plated film sample of plating titanium aln precipitation (TiAlN) hard reaction film places above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in the stripping liquid, does not contact with Glass Containers bottom and sidewall; In second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, metallic matrix color and metalluster before becoming plated film not; In the 3rd step, take out the plated film sample move back behind the film after 30 minutes; In the 4th step, move back plated film sample surfaces 2 minutes behind the film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample behind the film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back behind the film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light behind the film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back behind the film is consistent with uncoated metallic matrix, and detection is less than titanium (Ti), aluminium (Al), nitrogen (N) element.
Embodiment 2
The stripping method of the titanium-aluminum-zirconium nitride hard reaction film of plating on the stainless steel base
1, determining of stripping liquid raw material: determine gluconic acid sodium salt, NaOH, contain 30%H
2O
2Hydrogen peroxide, dodecyl sodium sulfate, sodium phosphate trimer, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step adds mass percent in the glass container and is 200 milliliters of 67.8% distilled water; Second step adds mass percent in the glass container and is 1.7% gluconic acid sodium salt 5 grams, stirs until fully dissolving; The 3rd step slowly added mass percent in the glass container and is 6.8% NaOH 20 grams, put the medicine rapid stirring on one side until whole the dissolving in course of dissolution, can discharge a certain amount of heat, caused that temperature slightly rises; The 4th step, be 0.4% dodecyl sodium sulfate (powder), 1.5 grams with mass percent with mass percent be that 0.3% sodium phosphate trimer (powder) 1 gram is composite, wherein, dodecyl sodium sulfate is 1:0.75 with the ratio of the mass fraction of sodium phosphate trimer, and the mass percent sum of the two is 0.7%, mixes, pour in the glass container, and the quick manual stirring, stop after 8 ~ 10 minutes stirring, naturally cool to room temperature; In the 5th step, add mass percent in the glass container and be 23% the 30%H that contains
2O
260 milliliters in hydrogen peroxide, wherein, NaOH with contain 30%H
2O
2The ratio of mass fraction of hydrogen peroxide be 1:3.4, and the mass percent sum of the two is 29.8%, stirs then, obtains stripping liquid.
3, determining of stripping technology: the first step, (thicknesses of layers is about 1.5 microns with plating titanium-aluminum-zirconium nitride (TiAlZrN) hard reaction film on the stainless steel base with Stainless Steel Wire, titanium, aluminium, zirconium, the nitrogen-atoms ratio is approximately Ti:Al:Zr:N=0.25:0.15:0.2:0.40) plated film sample (being of a size of 40 millimeters * 30 millimeters * 1 millimeter) be connected with anchor and fixing, wherein anchor places the Glass Containers top, the plated film sample of plating titanium-aluminum-zirconium nitride (TiAlZrN) hard reaction film places above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in the stripping liquid, does not contact with Glass Containers bottom and sidewall; In second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, metallic matrix color and metalluster before becoming plated film not; In the 3rd step, take out the plated film sample move back behind the film after 30 minutes; In the 4th step, move back plated film sample surfaces 2 minutes behind the film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample behind the film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back behind the film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light behind the film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back behind the film is consistent with uncoated metallic matrix, and detection is less than titanium (Ti), aluminium (Al), zirconium (Zr), nitrogen (N) element.
Embodiment 3
The stripping method of the titanium zirconium nitride hard reaction film of plating on the stainless steel base
1, determining of stripping liquid raw material: determine gluconic acid sodium salt, NaOH, contain 30%H
2O
2Hydrogen peroxide, dodecyl sodium sulfate, sodium phosphate trimer, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step adds mass percent in the glass container and is 200 milliliters of 63.8% distilled water; Second step adds mass percent in the glass container and is 3.2% gluconic acid sodium salt 10 grams, stirs until fully dissolving; The 3rd step slowly added mass percent in the glass container and is 9.6% NaOH 30 grams, put the medicine rapid stirring on one side until whole the dissolving in course of dissolution, can discharge a certain amount of heat, caused that temperature slightly rises; The 4th step, be 0.2% dodecyl sodium sulfate (powder), 0.5 gram with mass percent with mass percent be that 0.2% sodium phosphate trimer (powder) 0.5 gram is composite, wherein, dodecyl sodium sulfate is 1:1 with the ratio of the mass fraction of sodium phosphate trimer, and the mass percent sum of the two is 0.4%, mixes, pour in the glass container, and the quick manual stirring, stop after 8 ~ 10 minutes stirring, naturally cool to room temperature; In the 5th step, add mass percent in the glass container and be 23% the 30%H that contains
2O
265 milliliters in hydrogen peroxide, wherein, NaOH with contain 30%H
2O
2The ratio of mass fraction of hydrogen peroxide be 1:2.4, and the mass percent sum of the two is 32.6%, stirs then, obtains stripping liquid.
3, determining of stripping technology: the first step, (thicknesses of layers is about 1.5 microns with plating titanium zirconium nitride (TiZrN) hard reaction film on the stainless steel base with Stainless Steel Wire, titanium, zirconium, the nitrogen-atoms ratio is approximately Ti:Zr:N=0.35:0.25:0.40) plated film sample (being of a size of 40 millimeters * 30 millimeters * 1 millimeter) be connected with anchor and fixing, wherein anchor places the Glass Containers top, the plated film sample of plating titanium zirconium nitride (TiZrN) hard reaction film places above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in the stripping liquid, does not contact with Glass Containers bottom and sidewall; In second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, metallic matrix color and metalluster before becoming plated film not; In the 3rd step, take out the plated film sample move back behind the film after 120 minutes; In the 4th step, move back plated film sample surfaces 2 minutes behind the film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample behind the film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back behind the film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light behind the film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back behind the film is consistent with uncoated metallic matrix, and detection is less than titanium (Ti), zirconium (Zr), nitrogen (N) element.
Claims (1)
1. the stripping method of a multicomponent nitride hard reaction film is characterized in that: the steps include: determining of (1), stripping liquid raw material: determine gluconic acid sodium salt, NaOH, contain 30%H
2O
2Hydrogen peroxide, dodecyl sodium sulfate, sodium phosphate trimer, distilled water as the raw material of preparation stripping liquid; (2), the preparation of stripping liquid: the first step adds mass percent in the glass container and is 63.5% ~ 68% distilled water; Second step adds mass percent in the glass container and is 1.5% ~ 3.5% gluconic acid sodium salt, stirs until fully dissolving; The 3rd step slowly added mass percent in the glass container and is 6.5% ~ 10% NaOH, put the medicine rapid stirring on one side until whole the dissolving in course of dissolution, can discharge a certain amount of heat, caused that temperature slightly rises; The 4th step, be that 0.2% ~ 0.4% dodecyl sodium sulfate powder and mass percent are that 0.2% ~ 0.4% sodium phosphate trimer powder is composite with mass percent, wherein, the ratio of the mass fraction of dodecyl sodium sulfate and sodium phosphate trimer is between the 1:1 to 1:0.7, and the mass percent sum of the two must be in 0.4% ~ 0.8%, mixes then, pour in the glass container, and the quick manual stirring, stop after 8 ~ 10 minutes stirring, naturally cool to room temperature; In the 5th step, add mass percent in the glass container and be 20% ~ 25% the 30%H that contains
2O
2Hydrogen peroxide, wherein, NaOH with contain 30%H
2O
2The ratio of mass fraction of hydrogen peroxide be between the 1:3.5 to 1:2, and the mass percent sum of the two must be between 29% ~ 33%, stirs then, obtains stripping liquid; (3), determining of stripping technology: for sake of convenience, the sample of following plating multicomponent nitride hard reaction film is referred to as the plated film sample, the first step, the plated film sample is connected with fixed mount and fixing with stainless steel wire, wherein fixed mount places the glass container top, and the plated film sample places above-mentioned stripping liquid, keeps vertically, guarantee that simultaneously the plated film sample is soaked in the stripping liquid, not with glass container bottom and sidewall contact; Second step, the change color of the sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metallic luster of plated film; In the 3rd step, plated film sample behind the film is moved back in the rear taking-up that reacts completely of the rete of sample surfaces to be coated, that is, stripping TiAlN film and TiAlZrN film time are 30 minutes; The stripping TiZrN film time is 120 minutes; In the 4th step, move back plated film sample surfaces 2 minutes behind the film with distilled water flushing; In the 5th step, adopt absolute ethyl alcohol to clean to move back plated film sample behind the film after 1 minute and dry up.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103556164A (en) * | 2013-10-28 | 2014-02-05 | 沈阳大学 | Desizing method of titanium aluminum chromium nitride hard reaction film |
| CN103882459A (en) * | 2014-03-31 | 2014-06-25 | 沈阳大学 | Method for removing titanium chromium nitride hard reaction film |
| CN109576723A (en) * | 2019-01-29 | 2019-04-05 | 苏州涂冠镀膜科技有限公司 | Stripping cobalt base hard alloy surface nitride film layer moves back film liquid and method |
| CN109576719A (en) * | 2019-01-09 | 2019-04-05 | 株洲华锐精密工具股份有限公司 | A kind of hard coat is with moving back masking liquid and the preparation method and application thereof |
| CN115245920A (en) * | 2021-04-28 | 2022-10-28 | 潍坊华光光电子有限公司 | Cleaning method for semiconductor laser coating clamp |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103556164A (en) * | 2013-10-28 | 2014-02-05 | 沈阳大学 | Desizing method of titanium aluminum chromium nitride hard reaction film |
| CN103556164B (en) * | 2013-10-28 | 2015-08-19 | 沈阳大学 | A kind of obstacles in quit of titanium aluminium chromium nitride hard reaction film |
| CN103882459A (en) * | 2014-03-31 | 2014-06-25 | 沈阳大学 | Method for removing titanium chromium nitride hard reaction film |
| CN103882459B (en) * | 2014-03-31 | 2016-05-25 | 沈阳大学 | A kind of stripping method of titanium chromium nitride hard reaction film |
| CN109576719A (en) * | 2019-01-09 | 2019-04-05 | 株洲华锐精密工具股份有限公司 | A kind of hard coat is with moving back masking liquid and the preparation method and application thereof |
| CN109576723A (en) * | 2019-01-29 | 2019-04-05 | 苏州涂冠镀膜科技有限公司 | Stripping cobalt base hard alloy surface nitride film layer moves back film liquid and method |
| CN115245920A (en) * | 2021-04-28 | 2022-10-28 | 潍坊华光光电子有限公司 | Cleaning method for semiconductor laser coating clamp |
| CN115245920B (en) * | 2021-04-28 | 2024-02-06 | 潍坊华光光电子有限公司 | Cleaning method of semiconductor laser coating clamp |
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