CN102277587B - 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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- CN102277587B CN102277587B CN 201110214822 CN201110214822A CN102277587B CN 102277587 B CN102277587 B CN 102277587B CN 201110214822 CN201110214822 CN 201110214822 CN 201110214822 A CN201110214822 A CN 201110214822A CN 102277587 B CN102277587 B CN 102277587B
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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 is mainly titanium nitride (TiN), develops into gradually the multicomponent nitride hard reaction films such as TiAlN (TiAlN), titanium nitride zirconium (TiZrN) and TiAlN zirconium (TiAlZrN).Yet, due to the surface treatment of plating piece, many-sided reasons such as control of vacuum plating process, the not good situation of coating quality can appear often, such as, hardness is not high enough, sticking power is strong, rete local shedding etc.In case such situation occurs, 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 workpiece surface of cleaning.This just requires 2 points, and the first, original coatings stripping is clean; The second, keep moving back workpiece surface after film smooth and without evidence of corrosion, machinery-free scratch.
At present, the main method of stripping poor quality's rete is: 1, mechanical polishing, the method is only applicable to the workpiece that surface shape is simple, be easy to grinding and polishing, the surface complicated a little for shape is difficult to carry out, in addition, in polishing process, the situation that rete is difficult to strip fully or scratch workpiece surface easily appears; 2, chemistry stripping is mainly 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
A kind of stripping method that the purpose of this invention is to provide 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 Sunmorl N 60S, sodium hydroxide, contain 30%H
2O
2Hydrogen peroxide, sodium laurylsulfonate, tripoly phosphate sodium STPP, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step, adding mass percent in the Glass Containers is 63.5% ~ 68% distilled water; Second step, adding mass percent in the Glass Containers is 1.5% ~ 3.5% Sunmorl N 60S, stirs until dissolving fully; In the 3rd step, slowly adding mass percent in the Glass Containers is 6.5% ~ 10% sodium hydroxide, puts the medicine rapid stirring on one side until whole the dissolving in dissolution process, can discharge a certain amount of heat, causes that temperature slightly rises; The 4th step, be that 0.2% ~ 0.4% sodium laurylsulfonate powder and mass percent are that 0.2% ~ 0.4% tripoly phosphate sodium STPP powder is composite with mass percent, wherein, the ratio of the massfraction of sodium laurylsulfonate and tripoly phosphate sodium STPP is between 1:1 to 1:0.7, and mass percent sum both must be in 0.4% ~ 0.8%, then mixes, and pours in Glass Containers, and quick manual stirs and to stop after 8 ~ 10 minutes stirring, and naturally cools to room temperature; In the 5th step, adding mass percent in the Glass Containers is 20% ~ 25% the 30%H that contains
2O
2Hydrogen peroxide, wherein, sodium hydroxide with contain 30%H
2O
2The ratio of massfraction of hydrogen peroxide be between 1:3.5 to 1:2, and mass percent sum both must be between 29% ~ 33%, then stirs, and obtains stripping liquid.
3, determining of stripping technique: 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, with Stainless Steel Wire, the plated film sample is connected with anchor and fixes, wherein anchor is placed in above Glass Containers, and the plated film sample is placed in above-mentioned stripping liquid, keeps vertically, guarantee that simultaneously the plated film sample is soaked in stripping liquid, not with Glass Containers bottom and sidewall contact; Second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metalluster of plated film; In the 3rd step, plated film sample after 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 after film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample after 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 metallic matrix fully, thicknesses of layers is approximately 1.5 microns ~ 2 microns, move back the plated film sample surfaces light after film, has metalluster, and the employing energy spectrum analysis, the plated film sample surfaces composition that moves back after film is consistent with uncoated metallic matrix, can't detect titanium (Ti), aluminium (Al), zirconium (Zr), nitrogen (N) element; The stripping technique that the present invention proposes is simple and clear, easy handling; Determine the mass percent scope of a moiety in 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 stainless steel base
1, determining of stripping liquid raw material: determine Sunmorl N 60S, sodium hydroxide, contain 30%H
2O
2Hydrogen peroxide, sodium laurylsulfonate, tripoly phosphate sodium STPP, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step, adding mass percent in the Glass Containers is 200 milliliters of 68% distilled water; Second step, adding mass percent in the Glass Containers is 2% Sunmorl N 60S 6 grams, stirs until dissolving fully; In the 3rd step, slowly adding mass percent in the Glass Containers is 8.5% sodium hydroxide 25 grams, puts the medicine rapid stirring on one side until whole the dissolving in dissolution process, can discharge a certain amount of heat, causes that temperature slightly rises; The 4th step, be that 0.3% sodium laurylsulfonate (powder) 1 gram and mass percent are that 0.2% tripoly phosphate sodium STPP (powder) 0.6 gram is composite with mass percent, wherein, sodium laurylsulfonate is 1:0.7 with the ratio of the massfraction of tripoly phosphate sodium STPP, and mass percent sum both is 0.5%, mixes, and pours in Glass Containers, and quick manual stirs and to stop after 8 ~ 10 minutes stirring, and naturally cools to room temperature; In the 5th step, adding mass percent in the Glass Containers is 21% the 30%H that contains
2O
255 milliliters, hydrogen peroxide, wherein, sodium hydroxide with contain 30%H
2O
2The ratio of massfraction of hydrogen peroxide be 1:2.5, and mass percent sum both is 29.5%, then stirs, and obtains stripping liquid.
3, determining of stripping technique: the first step, (thicknesses of layers is about 1.5 microns with plating titanium aln precipitation (TiAlN) hard reaction film on 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 fixes, wherein anchor is placed in above Glass Containers, the plated film sample of plating titanium aln precipitation (TiAlN) hard reaction film is placed in above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in stripping liquid, not with Glass Containers bottom and sidewall contact, second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metalluster of plated film, in the 3rd step, take out the plated film sample move back after film after 30 minutes, in the 4th step, move back plated film sample surfaces 2 minutes after film with distilled water flushing, in the 5th step, adopt dehydrated alcohol to clean to move back plated film sample after film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back after film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light after film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back after film is consistent with uncoated metallic matrix, can't detect titanium (Ti), aluminium (Al), nitrogen (N) element.
Embodiment 2
The stripping method of the titanium-aluminum-zirconium nitride hard reaction film of plating on stainless steel base
1, determining of stripping liquid raw material: determine Sunmorl N 60S, sodium hydroxide, contain 30%H
2O
2Hydrogen peroxide, sodium laurylsulfonate, tripoly phosphate sodium STPP, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step, adding mass percent in the Glass Containers is 200 milliliters of 67.8% distilled water; Second step, adding mass percent in the Glass Containers is 1.7% Sunmorl N 60S 5 grams, stirs until dissolving fully; In the 3rd step, slowly adding mass percent in the Glass Containers is 6.8% sodium hydroxide 20 grams, puts the medicine rapid stirring on one side until whole the dissolving in dissolution process, can discharge a certain amount of heat, causes that temperature slightly rises; The 4th step, be that 0.4% sodium laurylsulfonate (powder) 1.5 grams and mass percent are that 0.3% tripoly phosphate sodium STPP (powder) 1 gram is composite with mass percent, wherein, sodium laurylsulfonate is 1:0.75 with the ratio of the massfraction of tripoly phosphate sodium STPP, and mass percent sum both is 0.7%, mixes, and pours in Glass Containers, and quick manual stirs and to stop after 8 ~ 10 minutes stirring, and naturally cools to room temperature; In the 5th step, adding mass percent in the Glass Containers is 23% the 30%H that contains
2O
260 milliliters, hydrogen peroxide, wherein, sodium hydroxide with contain 30%H
2O
2The ratio of massfraction of hydrogen peroxide be 1:3.4, and mass percent sum both is 29.8%, then stirs, and obtains stripping liquid.
3, determining of stripping technique: the first step, (thicknesses of layers is about 1.5 microns with plating titanium-aluminum-zirconium nitride (TiAlZrN) hard reaction film on 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 fix, wherein anchor is placed in above Glass Containers, the plated film sample of plating titanium-aluminum-zirconium nitride (TiAlZrN) hard reaction film is placed in above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in stripping liquid, not with Glass Containers bottom and sidewall contact, second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metalluster of plated film, in the 3rd step, take out the plated film sample move back after film after 30 minutes, in the 4th step, move back plated film sample surfaces 2 minutes after film with distilled water flushing, in the 5th step, adopt dehydrated alcohol to clean to move back plated film sample after film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back after film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light after film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back after film is consistent with uncoated metallic matrix, can't detect 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 stainless steel base
1, determining of stripping liquid raw material: determine Sunmorl N 60S, sodium hydroxide, contain 30%H
2O
2Hydrogen peroxide, sodium laurylsulfonate, tripoly phosphate sodium STPP, distilled water as the raw material of preparation stripping liquid.
2, the preparation of stripping liquid: the first step, adding mass percent in the Glass Containers is 200 milliliters of 63.8% distilled water; Second step, adding mass percent in the Glass Containers is 3.2% Sunmorl N 60S 10 grams, stirs until dissolving fully; In the 3rd step, slowly adding mass percent in the Glass Containers is 9.6% sodium hydroxide 30 grams, puts the medicine rapid stirring on one side until whole the dissolving in dissolution process, can discharge a certain amount of heat, causes that temperature slightly rises; The 4th step, be that 0.2% sodium laurylsulfonate (powder) 0.5 gram and mass percent are that 0.2% tripoly phosphate sodium STPP (powder) 0.5 gram is composite with mass percent, wherein, sodium laurylsulfonate is 1:1 with the ratio of the massfraction of tripoly phosphate sodium STPP, and mass percent sum both is 0.4%, mixes, and pours in Glass Containers, and quick manual stirs and to stop after 8 ~ 10 minutes stirring, and naturally cools to room temperature; In the 5th step, adding mass percent in the Glass Containers is 23% the 30%H that contains
2O
265 milliliters, hydrogen peroxide, wherein, sodium hydroxide with contain 30%H
2O
2The ratio of massfraction of hydrogen peroxide be 1:2.4, and mass percent sum both is 32.6%, then stirs, and obtains stripping liquid.
3, determining of stripping technique: the first step, (thicknesses of layers is about 1.5 microns with plating titanium zirconium nitride (TiZrN) hard reaction film on 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 fix, wherein anchor is placed in above Glass Containers, the plated film sample of plating titanium zirconium nitride (TiZrN) hard reaction film is placed in above-mentioned stripping liquid, keep vertically, guarantee that simultaneously the plated film sample is soaked in stripping liquid, not with Glass Containers bottom and sidewall contact, second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metalluster of plated film, in the 3rd step, take out the plated film sample move back after film after 120 minutes, in the 4th step, move back plated film sample surfaces 2 minutes after film with distilled water flushing, in the 5th step, adopt dehydrated alcohol to clean to move back plated film sample after film after 1 minute and dry up.
The plated film sample that uses aforesaid method to move back after film is carried out visual inspection, and rete strips fully, and moves back the plated film sample surfaces light after film, has metalluster.Adopt energy spectrum analysis, the plated film sample surfaces composition that moves back after film is consistent with uncoated metallic matrix, can't detect 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 Sunmorl N 60S, sodium hydroxide, contain 30%H
2O
2Hydrogen peroxide, sodium laurylsulfonate, tripoly phosphate sodium STPP, distilled water as the raw material of preparation stripping liquid; (2), the preparation of stripping liquid: the first step, adding mass percent in the Glass Containers is 63.5% ~ 68% distilled water; Second step, adding mass percent in the Glass Containers is 1.5% ~ 3.5% Sunmorl N 60S, stirs until dissolving fully; In the 3rd step, slowly adding mass percent in the Glass Containers is 6.5% ~ 10% sodium hydroxide, puts the medicine rapid stirring on one side until whole the dissolving in dissolution process, can discharge a certain amount of heat, causes that temperature slightly rises; The 4th step, be that 0.2% ~ 0.4% sodium laurylsulfonate powder and mass percent are that 0.2% ~ 0.4% tripoly phosphate sodium STPP powder is composite with mass percent, wherein, the ratio of the massfraction of sodium laurylsulfonate and tripoly phosphate sodium STPP is between 1:1 to 1:0.7, and mass percent sum both must be in 0.4% ~ 0.8%, then mixes, and pours in Glass Containers, and quick manual stirs and to stop after 8 ~ 10 minutes stirring, and naturally cools to room temperature; In the 5th step, adding mass percent in the Glass Containers is 20% ~ 25% the 30%H that contains
2O
2Hydrogen peroxide, wherein, sodium hydroxide with contain 30%H
2O
2The ratio of massfraction of hydrogen peroxide be between 1:3.5 to 1:2, and mass percent sum both must be between 29% ~ 33%, then stirs, and obtains stripping liquid; (3), determining of stripping technique: 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, with Stainless Steel Wire, the plated film sample is connected with anchor and fixes, wherein anchor is placed in above Glass Containers, and the plated film sample is placed in above-mentioned stripping liquid, keeps vertically, guarantee that simultaneously the plated film sample is soaked in stripping liquid, not with Glass Containers bottom and sidewall contact; Second step, the colour-change of the plated film sample surfaces that detects by an unaided eye can find that color shoals gradually, until become not front metallic matrix color and the metalluster of plated film; In the 3rd step, plated film sample after 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 after film with distilled water flushing; In the 5th step, adopt dehydrated alcohol to clean to move back plated film sample after film after 1 minute and dry up.
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| 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 |
| 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 |
| CN109576723B (en) * | 2019-01-29 | 2020-08-28 | 苏州涂冠镀膜科技有限公司 | Film stripping liquid and method for removing nitride film on surface of cobalt-based hard alloy |
| 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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