阅读说明：本技术 一种玻璃与不锈钢封装工件的钝化方法 (Passivation method for glass and stainless steel packaged workpiece ) 是由 马海军 胡昆鹏 左卫萍 于 2020-11-16 设计创作，主要内容包括：本发明涉及金属表面处理方法领域,尤其涉及一种玻璃与不锈钢封装工件的钝化方法；通过改进不锈钢件和玻璃制成复合件的封装方法,并结合钝化技术和封闭技术联合用于封装玻璃的不锈钢组合件上,可大大提升玻璃与不锈钢封装工件的整体防腐性能,使制得的玻璃与不锈钢封装工件进行中性盐雾测试,经过96小时测试时间工件仍然没有生锈。(The invention relates to the field of metal surface treatment methods, in particular to a passivation method for glass and stainless steel packaged workpieces; by improving the packaging method of the composite member made of the stainless steel member and the glass and combining the passivation technology and the sealing technology to be used for packaging the stainless steel assembly of the glass, the integral corrosion resistance of the glass and the stainless steel packaging workpiece can be greatly improved, so that the prepared glass and the stainless steel packaging workpiece are subjected to a neutral salt spray test, and the workpiece is still not rusted after 96 hours of testing.)

1. A passivation method for glass and stainless steel packaged workpieces is characterized by comprising the following steps:

carrying out pre-oxidation treatment on the stainless steel piece;

packaging glass on the stainless steel piece subjected to pre-oxidation treatment to obtain a stainless steel and glass composite assembly;

carrying out oxidation film removal treatment on the composite assembly;

carrying out plane grinding on the composite assembly subjected to the oxide film removal treatment;

cleaning the composite assembly after plane grinding;

carrying out vacuum passivation or chemical passivation on the cleaned composite assembly;

the vacuum passivation adopts an inductively coupled plasma chemical vapor deposition process and an in-furnace AF process, an ICP optical coating process is adopted to prime a vacuum passivation film, and then a layer of AF fingerprint-resistant film is coated by a vacuum evaporation coating process; the chemical passivation is carried out by selective chromate passivation treatment;

and sealing the composite assembly after vacuum passivation or chemical passivation to obtain a finished product.

2. The method for passivating a glass and stainless steel encapsulated workpiece as claimed in claim 1, wherein said pre-oxidation treatment specifically comprises the steps of:

the stainless steel piece is put into a degreasing furnace and is burnt for 4 to 6 hours in the air atmosphere at the temperature of 400-500 ℃.

3. The method for passivating a glass and stainless steel encapsulated workpiece as claimed in claim 1, wherein said pre-oxidation treatment specifically comprises the steps of:

putting the stainless steel part into a degreasing furnace, heating the degreasing furnace from normal temperature to 400-500 ℃ in an air atmosphere, and using for 60-100 minutes; preserving the heat for 60-90 minutes at the temperature of 400-; cooling from 400-500 deg.c to room temperature for 60-90 min.

4. The passivation method of glass and stainless steel packaged workpieces according to claim 1, wherein the step of packaging the glass on the stainless steel member subjected to the pre-oxidation treatment to obtain the stainless steel and glass composite assembly comprises the following steps:

packaging the stainless steel piece subjected to the pre-oxidation treatment and the glass in a continuous furnace with the atmosphere of 85% argon and 15% hydrogen or a batch furnace with the atmosphere of nitrogen according to the following conditions to obtain a stainless steel and glass composite assembly:

raising the temperature from normal temperature to 800-950 ℃ for 2-3 hours;

keeping the temperature at 800 ℃ and 950 ℃ for 1-1.5 hours;

cooling from 800 ℃ to 950 ℃ to 500 ℃ to 550 ℃ for 2-2.5 hours;

preserving the heat for 0.5 to 1 hour at the temperature of 500-550 ℃;

reducing the temperature from 500-550 ℃ to 400-450 ℃ for 1.5-2 hours;

cooling from 400-450 ℃ to normal temperature for 1.5-2 hours.

5. The method of claim 1, wherein the performing an oxide film removal process on the composite assembly comprises: soaking the composite component for 3-5 minutes at 20-30 ℃ by using a film remover, and then carrying out centrifugal grinding or magnetic grinding on the composite component, wherein the film remover comprises the following raw materials in parts by weight: 3-5 parts of citric acid; 25-35 parts of hydrogen peroxide; 1-2 parts of organic brightening agent.

6. The method of claim 1, wherein the step of performing a surface polishing on the composite assembly after the oxide film removal process comprises the steps of:

roughing the composite component by using a sand skin, wherein the grinding liquid is clear water, and the grinding time is 3-6 minutes;

performing middle polishing treatment on the coarsely-opened composite assembly for 20-30 minutes by using middle polishing liquid of red cerium oxide middle polishing skin and aluminum oxide as an abrasive;

and (3) performing fine polishing treatment on the composite component after the middle polishing for 5-10 minutes by adopting black fine polishing skin and using aluminum oxide as a fine polishing liquid of an abrasive material.

7. The method for passivating a glass and stainless steel encapsulated workpiece as claimed in claim 1, wherein said cleaning of the planar ground composite assembly specifically comprises the steps of:

the ultrasonic wax removal cleaning is carried out by adopting a wax removal agent with the concentration of 10-15%, wherein the wax removal agent comprises the following ingredients in parts by weight: 15-20 parts of fatty alcohol-polyoxyethylene ether, 12-18 parts of alkaline oil, 22-27 parts of triethanolamine and 13-17 parts of oleic acid, wherein the cleaning temperature is 80-90 ℃;

after ultrasonic wax removal cleaning, ultrasonic oil removal cleaning is carried out by adopting an oil removal agent with the concentration of 10-15%, wherein the oil removal agent comprises the following ingredients in parts by weight: 6-11 parts of fatty alcohol-polyoxyethylene ether, 8-13 parts of nonionic active agent, 10-15 parts of sodium carbonate, 8-12 parts of surfactant and 5-10 parts of sodium tripolyphosphate, and the cleaning temperature is 80-90 ℃;

after ultrasonic degreasing and cleaning, performing ultrasonic high-brightness cleaning by using a high-brightness cleaning agent with the concentration of 10-15%, wherein the high-brightness cleaning agent is composed of the following ingredients in parts by weight: 8-13 parts of sodium polyphosphate, 15-20 parts of surfactant, 3-8 parts of citric acid and 2-7 parts of auxiliary agent;

after ultrasonic high-brightness cleaning, slow-pulling water cleaning is carried out, the slow-pulling temperature is 80-90 ℃, the time is 80-120s, and the conductivity is less than 20 mu m/cm;

after slow-pulling and water washing, baking at 60-80 ℃ for 8-15 min.

8. The method for passivating a glass and stainless steel encapsulated workpiece according to claim 1, wherein the sealing treatment specifically comprises:

treating with an aqueous sealant, wherein the aqueous sealant is a nickel protective agent, the concentration of the nickel protective agent is 3-5%, the treatment temperature is 50-60 ℃, and the treatment time is 3-5 minutes;

AF treatment, wherein the main components of the AF nano oil used in the AF treatment are perfluoropolyether and nano silicon dioxide.

Technical Field

The invention relates to the field of metal surface treatment methods, in particular to a passivation method for a glass and stainless steel packaged workpiece.

Background

Cr is the most main alloy element in stainless steel, and can form a stable and compact chromium oxide protective inner-layer metal matrix on the alloy surface layer. Generally, the standard potential of the metal on the surface layer is transited from-0.4V to 0.5-1.0V through passivation, the activation energy of the anode reaction is obviously increased, and the inert oxidation reaction is shown. This property of the Cr element is the basis for achieving high corrosion resistance of stainless steel materials in corrosive media, a phenomenon known as a passivating effect of the metal. The stainless steel further forms various passivation layers under additional conditions to further improve the corrosion resistant effect, namely the passivation process of the stainless steel.

At present, in the field of passivation, the passivation technology of a single stainless steel material is mature, an artificial passivation method mainly comprises electrochemical passivation and chemical passivation, the electrochemical passivation is to make the anode of the stainless steel material polarized by an external current, the dissolution rate of the stainless steel is rapidly reduced, high stability is kept in a certain range, and a stainless steel workpiece subjected to electrochemical passivation has better corrosion resistance; the chemical passivation is mainly to form a layer of passivation film on the surface of the workpiece. For the passivation process of stainless steel, the passivation process mainly has 3 characteristics from the chemical reaction of the formation of the passivation process, wherein (1) water molecules directly participate in the formation of a passivation film, and the passivant exists in the form of solution and is a necessary condition for passivation formation; (2) the passivation process of the metal surface is the result of the combined action of several reactions, including the growth process of the passivation layer and the dissolution reaction of the metal; (3) a passivation film is present on the passivated metal surface. However, the nature of the passivation film is not yet determined. The most representative of these theories are the phase-forming film theory and the adsorption film theory. Researchers tend to think now that passivation phenomenon can be explained by combining the theory of phase-forming film and the theory of adsorption, wherein the formation of adsorption film determines the difficulty of passivation, and oxygen-containing particles play a dominant role in the initial stage of passivation on the surface of stainless steel; as the passivation process continues, the initially formed adsorption film gradually develops into a phase-forming film, which plays a dominant role in maintaining the passivation state. The passivation technology aiming at the stainless steel mainly comprises the following systems: 1. inorganic passivation system: such as nitric acid, chromic acid, hydrochloric acid, sulfuric acid, silicate, rare earth metal salt, molybdate, tungstate, hydrogen peroxide and other passivation systems; 2. organic passivation system: such as citric acid, phytic acid, silane coupling agents, fluoroalkanes, and the like; organic-inorganic composite passivation systems can be broadly classified into "composite passivation of silane and inorganic salt" and "composite passivation of polymer resin and inorganic salt" 2 categories.

The passivation technology of a single stainless steel material is mature, however, the corrosion resistance of an assembly packaged by stainless steel and glass is greatly reduced, and the position where rust is generated in a salt spray test is always concentrated at the interface of the glass and the stainless steel, and the main reasons are concentrated in the following points: 1. various atoms in the glass and the stainless steel can migrate and mutually permeate in the high-temperature packaging process, so that the chromium content in the stainless steel position near the interface of the glass and the stainless steel is reduced, and the corrosion resistance is reduced; 2. a pre-oxidation process is provided for increasing wettability of glass and stainless steel before glass packaging, and oxide film (mainly comprising ferric oxide, chromic oxide, and compact spinel-structured ferroferric oxide, NiO. Cr) remained in the gap between glass and stainless steel after glass packaging₂O₃) In addition, after the processes of rust removal and mirror polishing, the clearance between the glass and the stainless steel is added with the impurity particles such as aluminum oxide, silicon dioxide and the like in the grinding fluid, and the impurity particles are difficult to remove completely, so that chloride ions in the salt water penetrate into the clearance to react with the impurity particles in the salt spray test process after passivation, and the salt spray rust is caused; 3. the reason why 24H is difficult to do is found that the single stainless steel and the single glass are mainly two different materials, the thermal expansion coefficients of the stainless steel and the glass are different to cause poor air tightness after packaging, and a corrosive medium in the salt spray test process can pass over 96 hours(water, oxygen, chloride ions and the like) can permeate into the surface of the stainless steel substrate through the position with defective air tightness under the capillary action, and as time lengthens, a corrosion medium continuously permeates to the substrate through pores and chemically corrodes the substrate.

In summary, stainless steel assemblies of encapsulated glass processed by existing passivation processes have not achieved satisfactory corrosion protection in the passivation industry.

Disclosure of Invention

The technical problem to be solved by the invention is as follows: provides a passivation process of a stainless steel assembly for packaging glass, which aims to solve the problem that the glass and stainless steel composite assembly is easy to corrode.

The invention relates to a passivation method of a glass and stainless steel packaging workpiece, which comprises the following steps:

carrying out pre-oxidation treatment on the stainless steel piece;

packaging glass on the stainless steel piece subjected to pre-oxidation treatment to obtain a stainless steel and glass composite assembly;

carrying out oxidation film removal treatment on the composite assembly;

carrying out plane grinding on the composite assembly subjected to the oxide film removal treatment;

cleaning the composite assembly after plane grinding;

carrying out vacuum passivation or chemical passivation on the cleaned composite assembly;

the vacuum passivation adopts an inductively coupled plasma chemical vapor deposition process and an in-furnace AF process, an ICP optical coating process is adopted to prime a vacuum passivation film, and then a layer of AF fingerprint-resistant film is coated by a vacuum evaporation coating process; the chemical passivation is carried out by selective chromate passivation treatment;

and sealing the composite assembly after vacuum passivation or chemical passivation to obtain a finished product.

The invention has the beneficial effects that: in the passivation method for the glass and stainless steel packaged workpiece, the whole corrosion resistance of the glass and stainless steel packaged workpiece can be greatly improved by improving the packaging method for manufacturing the composite part by the stainless steel part and the glass and combining the passivation technology and the sealing technology to be used for packaging the stainless steel assembly of the glass, so that the manufactured glass and stainless steel packaged workpiece are subjected to a neutral salt spray test, and the workpiece is still not rusted after 96H test time.

Detailed Description

In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.

The invention relates to a passivation method of a glass and stainless steel packaging workpiece, which comprises the following steps:

carrying out pre-oxidation treatment on the stainless steel piece;

packaging glass on the stainless steel piece subjected to pre-oxidation treatment to obtain a stainless steel and glass composite assembly;

carrying out oxidation film removal treatment on the composite assembly;

carrying out plane grinding on the composite assembly subjected to the oxide film removal treatment;

cleaning the composite assembly after plane grinding;

carrying out vacuum passivation or chemical passivation on the cleaned composite assembly;

the vacuum passivation adopts an inductively coupled plasma chemical vapor deposition process and an in-furnace AF process, an ICP optical coating process is adopted to prime a vacuum passivation film, and then a layer of AF fingerprint-resistant film is coated by a vacuum evaporation coating process; the chemical passivation is carried out by selective chromate passivation treatment;

and sealing the composite assembly after vacuum passivation or chemical passivation to obtain a finished product.

In the method, glass and a stainless steel part are packaged and combined together, then the combined composite assembly is passivated, and the passivated composite assembly is subjected to sealing treatment to obtain a finished product, wherein after the composite assembly subjected to plane grinding is cleaned, laser etching can be performed on the composite assembly subjected to the cleaning step, and marks such as laser etching Logo and waterproof performance requirements are specifically used; after laser engraving and before passivation, the composite component can be subjected to passivation pretreatment, the passivation pretreatment modes mainly comprise cold removal treatment, vacuum film removal cleaning, crack cleaning agent cleaning, wax removal, oil removal and cleaning and the like, the cold remover is a solvent emulsion type degreasing and degreasing oil remover, the cold remover consists of an organic solvent and a surfactant and has a good stripping effect on heavy oil stains and dry solid oil stains on the surface of a metal material, and the cold remover with the best effect is kerosene; the vacuum film removal cleaning refers to oil removal cleaning in a vacuum state, so that impurities in gaps are more easily pulled out; the crack cleaning agent is an acidic liquid medicine containing organic acids such as nicotinic acid, sulfamic acid and the like and specially used for cleaning gaps, and has the effects of activation and hole expansion; wax and oil removal cleaning is the most conventional cleaning mode, ultrasonic waves are needed to be matched, the ultrasonic frequency can be 24kHz, 40kHz, 80kHz and 120kHz, and the higher the ultrasonic frequency is, the better the cleaning effect on gaps is.

In the passivation method for the glass and stainless steel packaged workpiece, the overall corrosion resistance of the glass and stainless steel packaged workpiece can be greatly improved by improving the packaging method of the stainless steel part and the glass made composite part and combining the passivation technology and the sealing technology to be used for packaging the glass stainless steel assembly.

Further, in the passivation method of the glass and stainless steel packaged workpiece, the pre-oxidation treatment specifically comprises the following steps:

the stainless steel piece is put into a degreasing furnace and is burnt for 4 to 6 hours in the air atmosphere at the temperature of 400-500 ℃.

Further, in the passivation method of the glass and stainless steel packaged workpiece, the pre-oxidation treatment specifically comprises the following steps:

putting the stainless steel part into a degreasing furnace, heating the degreasing furnace from normal temperature to 400-500 ℃ in an air atmosphere, and using for 60-100 minutes; preserving the heat for 60-90 minutes at the temperature of 400-; cooling from 400-500 deg.c to room temperature for 60-90 min.

As can be seen from the above description, the stainless steel is subjected to the pre-oxidation treatment to form an oxide layer on the surface, and the wettability of the liquid glass on the surface of the oxide layer is improved. The wettability reflects the binding capacity between two substances, and the concept of wetting can be used as the theoretical basis of the packaging process, because the sealing of glass and metal is actually a surface wetting problem, and a layer of porous oxide film is generated on the surface of a workpiece; the surface of the stainless steel is subjected to preoxidation treatment to form low-valent oxide, metal ions can form the maximum binding force and the minimum repulsive force with positive and negative ions in glass, and in addition, the liquid glass and the oxide layer on the surface of the stainless steel are mutually fused and diffused to form a stronger polar bond, so that the oxide layer can promote the wetting of the glass and the stainless steel.

Further, in the passivation method of the glass and stainless steel packaged workpiece, the step of packaging the glass on the stainless steel member subjected to the pre-oxidation treatment to obtain the stainless steel and glass composite assembly specifically comprises the following steps:

packaging the stainless steel piece subjected to the pre-oxidation treatment and the glass in a continuous furnace with the atmosphere of 85% argon and 15% hydrogen or a batch furnace with the atmosphere of 100% nitrogen according to the following conditions to obtain a stainless steel and glass composite assembly:

raising the temperature from normal temperature to 800-950 ℃ for 2-3 hours;

keeping the temperature at 800 ℃ and 950 ℃ for 1-1.5 hours;

cooling from 800 ℃ to 950 ℃ to 500 ℃ to 550 ℃ for 2-2.5 hours;

preserving the heat for 0.5 to 1 hour at the temperature of 500-550 ℃;

reducing the temperature from 500-550 ℃ to 400-450 ℃ for 1.5-2 hours;

cooling from 400-450 ℃ to normal temperature for 1.5-2 hours.

From the above description, the atmosphere, temperature, holding time, temperature rise time and fall time in the packaging process are all very important, for example, the packaging failure is caused by too large temperature gradient in the packaging process, too much thermal shock is caused to the packaging piece when the furnace is heated up or cooled down, too large difference of expansion coefficients of glass and metal can cause packaging failure, poor air tightness can easily occur when the packaging is not good, the gap between the glass and the stainless steel can be easily stored with dirt and dirt due to poor air tightness, and corrosive media (water, oxygen, chloride ions and the like) can permeate into the surface of the stainless steel substrate through the position with the defect air tightness under the capillary action to react with iron to generate iron rust in the salt spray test process, so that the salt spray test is NG.

Further, in the passivation method for glass and stainless steel packaged workpieces, the step of performing an oxide film removal treatment on the composite assembly specifically comprises: soaking the composite component for 3-5 minutes at 20-30 ℃ by using a film remover, and then carrying out centrifugal grinding or magnetic grinding on the composite component, wherein the film remover comprises the following raw materials in parts by weight: 3-5 parts of citric acid; 25-35 parts of hydrogen peroxide; 1-2 parts of organic brightening agent.

As can be seen from the above description, the film remover is an acidic liquid medicine containing no hydrofluoric acid and hydrochloric acid, and further derusting is carried out by centrifugal grinding or magnetic grinding after derusting. The surface of the stainless steel glass sealing member after sintering forms a layer of gray black oxide film, and the main components of the oxide film are ferric oxide, chromic oxide, ferroferric oxide with compact spinel structure, NiO & Cr₂O₃The oxide film is difficult to remove, and the subsequent processing and use are influenced. The subsequent salt spray is greatly influenced by the process of rust removal, the hydrofluoric acid can corrode glass, the hydrochloric acid can react with chromium in the stainless steel to reduce the chromium content, the corrosion resistance of the stainless steel can be reduced due to the reduction of the chromium content, and meanwhile, the hydrochloric acid can react with the stainless steel to cause poor air tightness, so that the development of a rust remover which does not harm the glass and does not influence the air tightness is very critical.

Further, in the passivation method of the glass and stainless steel packaged workpiece, the step of performing plane grinding on the composite assembly subjected to the oxide film removal treatment specifically comprises the following steps:

roughing the composite component by using a sand skin, wherein the grinding liquid is clear water, and the grinding time is 3-6 minutes;

performing middle polishing treatment on the coarsely-opened composite assembly for 20-30 minutes by using middle polishing liquid of red cerium oxide middle polishing skin and aluminum oxide as an abrasive;

and (3) performing fine polishing treatment on the composite component after the middle polishing for 5-10 minutes by adopting black fine polishing skin and fine polishing liquid which adopts alumina or silicon oxide as an abrasive material.

As can be seen from the above description, the equipment used in this step is a flat grinding machine, which mainly comprises three steps of rough polishing, middle polishing and fine polishing, and the polishing liquid can be a polishing liquid using silicon dioxide as an abrasive or a polishing liquid using aluminum oxide as an abrasive.

Further, in the passivation method of the glass and stainless steel packaged workpiece, the step of cleaning the composite assembly after plane grinding specifically comprises the following steps:

the ultrasonic wax removal cleaning is carried out by adopting a wax removal agent with the concentration of 10-15%, wherein the wax removal agent comprises the following ingredients in parts by weight: 15-20 parts of fatty alcohol-polyoxyethylene ether, 12-18 parts of alkaline oil, 22-27 parts of triethanolamine and 13-17 parts of oleic acid, wherein the cleaning temperature is 80-90 ℃;

after ultrasonic wax removal cleaning, ultrasonic oil removal cleaning is carried out by adopting an oil removal agent with the concentration of 10-15%, wherein the oil removal agent comprises the following ingredients in parts by weight: 6-11 parts of fatty alcohol-polyoxyethylene ether, 8-13 parts of nonionic active agent, 10-15 parts of sodium carbonate, 8-12 parts of surfactant and 5-10 parts of sodium tripolyphosphate, and the cleaning temperature is 80-90 ℃;

after ultrasonic degreasing and cleaning, carrying out ultrasonic high-brightness cleaning by adopting an acidic high-brightness cleaning agent with the concentration of 10-15%, wherein the acidic high-brightness cleaning agent is composed of the following ingredients in parts by weight: 8-13 parts of sodium polyphosphate, 15-20 parts of surfactant, 3-8 parts of citric acid and 2-7 parts of auxiliary agent;

after ultrasonic high-brightness cleaning, slow-pulling water cleaning is carried out, the slow-pulling temperature is 80-90 ℃, the time is 80-120S, and the conductivity is less than 20 mu m/cm;

after slow-pulling and water washing, baking at 60-80 ℃ for 6-15 min.

From the above description, it can be known that the cleaning after flat grinding has a great influence on the salt spray, and especially, the grinding fluid and the abrasive material hidden in the gap between the glass and the stainless steel are not cleaned thoroughly, which may cause chloride ions, water and oxygen in the salt water to permeate into the gap to react with these impurity particles during the salt spray testing process after passivation, thereby causing the salt spray to rust.

The following is a specific post-flat-grinding cleaning process:

1. ultrasonic hot water washing

A tank No. 1, in which a paraffin removal agent BTO-2010 and pure water are used for dispensing, the temperature is 85 +/-5 ℃, the ultrasonic cleaning time is 3-5min, and the concentration is 12.5%;

adding the liquid medicine: 10L/day; maintenance cycle: the replacement is carried out once in 1 day; ultrasonic current: 2-4A;

2. ultrasonic wave wax removal

A No. 2 tank, namely an oil removing agent BTO-2010, a pure water dosage, 85 +/-5 ℃, 6-8min of ultrasonic cleaning time and 12.5% of concentration;

adding the liquid medicine: 10L/day; maintenance cycle: the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

groove # 3: ultrasonic washing with water at 65 + -5 deg.C for 2-3min, and adding tap water; the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

3. ultrasonic oil removal

4# groove, highlight cleaning agent BTO-2018, pure water dosage, 85 plus or minus 5 ℃, ultrasonic cleaning time 6-8min, concentration 12.5%;

adding the liquid medicine: 10L/day; maintenance cycle: the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

5# groove: ultrasonic washing with water at 65 + -5 deg.C for 2-3min, and adding tap water; the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

4. high-brightness cleaning agent

The No. 6 tank is BTO-3089, pure water is used for dispensing, the temperature is 85 +/-5 ℃, the ultrasonic cleaning time is 6-8min, and the concentration is 12.5%;

adding the liquid medicine: 10L/day; maintenance cycle: the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

7# groove: ultrasonic washing with water at 65 + -5 deg.C for 2-3min, and adding tap water; the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

groove # 8: spraying and washing with water at normal temperature for 30-60S;

9#, 10#, 11 #: washing with ultrasonic water at 65 + -5 deg.C for 1-2min, and purifying with pure water; once replacing for 4 days; ultrasonic current: 2-4A;

the conductivity is less than 0.05 ms/cm;

12#, 13# slot: washing with ultrasonic water at 65 + -5 deg.C for 1-2min, and purifying with pure water; the replacement is carried out once in 2 days; ultrasonic current: 2-4A;

the conductivity is less than 0.05 ms/cm;

5. slowly pulling

Groove # 14: pure water at 80-90 deg.C for 1-2 min; the replacement is carried out once per shift; the conductivity is less than 0.02 ms/cm;

6. drying by baking

Preheating: 50-60 ℃;

drying 1: 60-80 deg.C for 8-15 min;

further, in the passivation method of the glass and stainless steel packaged workpiece, the sealing treatment specifically comprises:

treating with an aqueous sealant, wherein the aqueous sealant is a nickel protective agent, the concentration of the nickel protective agent is 3-5%, the treatment temperature is 50-60 ℃, and the treatment time is 3-5 minutes;

AF treatment, wherein the main components of the AF nano oil used in the AF treatment are perfluoropolyether and nano silicon dioxide.

As can be seen from the above description, the perfluoropolyether mainly plays a hydrophobic role, and the nanosilicon dioxide has a filling effect on the gap between the glass and the stainless steel. The AF treatment comprises in-furnace AF treatment, soaking AF treatment and spraying AF treatment, wherein a process of soaking AF nano-oil twice can be selected, a process of soaking AF nano-oil firstly and then spraying AF nano-oil can be selected, and a process of spraying AF nano-oil firstly and then soaking AF nano-oil can be selected; the AF nano oil is particularly helpful to the salt spray test, and the thicker the nano oil is, the longer the salt spray resisting time is.

Example one

A passivation process for a glass and stainless steel sealing assembly comprises the following steps,

a-glass and stainless steel MIN piece are packaged and combined together; the method sequentially comprises the following steps:

a 1-manufacture of stainless steel MIN pieces: manufacturing a stainless steel MIN piece rough blank by adopting a conventional MIN piece processing technology;

A2-Pre-Oxidation: pre-oxidizing the MIN part;

a 3-encapsulating glass: packaging glass for the workpiece subjected to preoxidation treatment;

a4-derusting: carrying out oxidation film removing treatment on the stainless steel composite assembly packaged with the glass;

a5-mirror polishing: carrying out plane grinding on the workpiece subjected to the rust removal treatment to enable the surface of the workpiece to achieve a mirror surface effect;

a6-washing: cleaning the workpiece subjected to the flat grinding step;

a7-laser etching: carrying out front laser etching on the workpiece subjected to the cleaning step;

b-passivation pretreatment: cleaning the workpiece in the laser etching step before passivation to ensure that the gap between the glass and the stainless steel of the workpiece does not contain impurities as much as possible;

c-passivation: passivating the product cleaned by pretreatment.

D-blocking: and sealing the passivated product.

E-salt spray test: and (5) carrying out neutral salt spray test on the passivated workpiece.

Preferably, the processing equipment used in step a1 comprises a feeder, an injection molding machine, a degreasing furnace, a sintering furnace and a shaping machine, and sequentially comprises the following steps: feeding, injecting, sintering and shaping;

in this embodiment, the apparatus used in step a2 is a degreasing furnace.

In this embodiment, the apparatus used in step a3 is a batch sintering furnace.

Preferably, the film remover used in the step A4 is an acidic liquid medicine containing no hydrofluoric acid and hydrochloric acid, and further derusting is carried out through centrifugal grinding after derusting.

In this embodiment, the apparatus used in step a5 is a flat grinding machine, which mainly includes three steps of rough polishing, middle polishing and fine polishing, and the polishing liquid uses alumina as the polishing liquid of the abrasive.

Preferably, the step A6, the step A6 sequentially comprise the following steps:

a6-1, performing two ultrasonic wax removal steps, wherein the concentration of a liquid medicine is 13%, the temperature is 85 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 8; removing wax, ultrasonic hot water washing at 65 deg.C for 2 min;

a6-2, removing oil by ultrasonic waves, wherein the concentration of a liquid medicine is 12.5%, the temperature is 85 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 9; the oil removal is followed by ultrasonic hot water washing at 65 ℃ for 2 min;

a6-3, ultrasonic high-brightness cleaning, wherein the concentration of a liquid medicine is 15%, the temperature is 85 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 2; the highlight cleaning is followed by ultrasonic hot water washing at 65 ℃ for 2 min; then sequentially carrying out spray water washing and four ultrasonic hot water washing at the temperature of 65 ℃ for 2 min;

a6-4, slow-pull washing, wherein the slow-pull temperature is 85 ℃, the time is 120S, and the conductivity is less than 20 mu m/cm;

a6-5, baking at 65 ℃ for 10 min.

In this embodiment, the passivation pretreatment mode adopted in step B is conventional wax and oil removal, and ultrasonic waves are required to be used together, with an ultrasonic frequency of 40 kHz. Dewaxing at 85 deg.c and pH 9 for 3min, and ultrasonic current 3A; degreasing PH is 10, temperature is 75 ℃, time is 3 minutes, ultrasonic current is 3A.

Preferably, step C adopts chemical passivation, and mainly selects the chromate passivation treatment process with the strongest passivation capability, and the chromate passivation has strong self-repairing capability. The passivation step is mainly divided into two steps, wherein the first step is passivation, the concentration is stock solution, the temperature is 60 ℃, the time is 60 minutes, and the pH value is 1-2; the second step is coordination, the concentration is stock solution, the temperature is 55 ℃, the time is 30 minutes, and the pH value is 2-4. Coordination serves to enhance the passivation effect, and if only passivation is used alone, the salt spray effect is much worse.

Specifically, the step D comprises three steps, wherein in the first step, nickel protection is carried out, the concentration is 4%, the temperature is 50 ℃, the time is 5 minutes, and then the product is washed by water for 3 times and dried; the second step is to soak the nano oil for 10 minutes, the baking temperature is 160 ℃, and the baking time is 40 minutes; and the third step is to spray nanometer oil, the baking temperature is 160 ℃, and the baking time is 40 minutes.

And E, performing neutral salt spray test on the workpiece produced by the process, wherein the workpiece still does not rust after 96 hours of test.

Example two

The second embodiment is a further improvement of the first embodiment on the basis of the first embodiment on the steps a, B, C and E, and is different from the first embodiment in that: the packaging equipment used in the step A4 is a mesh belt furnace, and sequentially comprises the following steps:

preferably, the processing equipment used in step a1 comprises a feeder, an injection molding machine, a degreasing furnace, a sintering furnace and a shaping machine, and sequentially comprises the following steps: feeding, injecting, sintering and shaping;

in this embodiment, the apparatus used in step a2 is a degreasing furnace.

In this embodiment, the apparatus used in step A3 is a mesh belt furnace.

Preferably, the film remover used in the step A4 is an acidic liquid medicine containing no hydrofluoric acid and hydrochloric acid, and further derusting is carried out by magnetic grinding after derusting.

In this embodiment, the apparatus used in step a5 is a flat grinding machine, which mainly includes three steps of rough polishing, middle polishing and fine polishing, and the polishing liquid uses silicon dioxide as the polishing liquid of the abrasive.

Preferably, the step A6, the step A6 sequentially comprise the following steps:

a6-1, performing two ultrasonic wax removal steps, wherein the concentration of a liquid medicine is 12.5%, the temperature is 90 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 8; removing wax, ultrasonic hot water washing at 65 deg.C for 2 min;

a6-2, removing oil by ultrasonic waves, wherein the concentration of a liquid medicine is 12.5%, the temperature is 90 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 9; the oil removal is followed by ultrasonic hot water washing at 65 ℃ for 2 min;

a6-3, ultrasonic high-brightness cleaning, wherein the concentration of a liquid medicine is 15%, the temperature is 90 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 2; the highlight cleaning is followed by ultrasonic hot water washing at 65 ℃ for 2 min; then sequentially carrying out spray water washing and four ultrasonic hot water washing at the temperature of 65 ℃ for 2 min;

a6-4, slow-pull washing, wherein the slow-pull temperature is 80 ℃, the time is 120s, and the conductivity is less than 20 mu m/cm;

a6-5, baking at 70 ℃ for 8 min.

In this embodiment, the passivation pretreatment mode adopted in step B is to first adopt cold degreasing treatment (adopting kerosene soaking for 8H), and then adopt conventional wax and oil removal cleaning treatment, which needs to be matched with ultrasonic waves with an ultrasonic frequency of 40 kHz. Dewaxing at 85 deg.c and pH 9 for 3min, and ultrasonic current 3A; deoiling pH 10, temperature 75 deg.C, time 3min, ultrasonic current 3A.

Preferably, the chemical passivation is adopted in the step C, and the method is mainly divided into three steps of passivation, wherein the first passivation is performed at the concentration of stock solution for 20 minutes at the temperature RT and the pH value of 1-2; the second passivation concentration is the original solution, the time is 10 minutes, the temperature is RT, and the PH is 1-2; the third passivation concentration is the stock solution, time 60 minutes, temperature RT, pH 1-2.

Specifically, the step D comprises two steps, wherein the first step is to spray the nano oil, the baking temperature is 160 ℃, the baking time is 30 minutes, and the second step is to soak the nano oil, the soaking time is 10 minutes, the baking temperature is 160 ℃, and the baking time is 30 minutes.

And E, performing neutral salt spray test on the workpiece produced by the process, wherein the workpiece still does not rust after 96 hours of test.

EXAMPLE III

The third embodiment is different from the first and second embodiments in that: step C adopts a vacuum passivation process, while the first embodiment and the second embodiment both adopt a chemical passivation process, and the third embodiment sequentially comprises the following steps:

preferably, the processing equipment used in step a1 comprises a feeder, an injection molding machine, a degreasing furnace, a sintering furnace and a shaping machine, and sequentially comprises the following steps: feeding, injecting, sintering and shaping;

in this embodiment, the apparatus used in step a2 is a degreasing furnace.

In this embodiment, the apparatus used in step A3 is a batch furnace.

Preferably, the film remover used in the step A4 is an acidic liquid medicine containing no hydrofluoric acid and hydrochloric acid, and further derusting is carried out by magnetic grinding after derusting.

In this embodiment, the apparatus used in step a5 is a flat grinding machine, which mainly includes three steps of rough polishing, middle polishing and fine polishing, and the polishing liquid uses silicon dioxide as the polishing liquid of the abrasive.

Preferably, the step A6, the step A6 sequentially comprise the following steps:

a6-1, performing two ultrasonic wax removal steps, wherein the concentration of a liquid medicine is 13%, the temperature is 87 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 8; removing wax, ultrasonic hot water washing at 65 deg.C for 2 min;

a6-2, removing oil by ultrasonic waves, wherein the concentration of a liquid medicine is 13%, the temperature is 90 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 9; the oil removal is followed by ultrasonic hot water washing at 65 ℃ for 2 min;

a6-3, ultrasonic high-brightness cleaning, wherein the concentration of a liquid medicine is 13%, the temperature is 90 ℃, the time is 6min, the ultrasonic current is 4A, and the pH value is 2; the highlight cleaning is followed by ultrasonic hot water washing at 65 ℃ for 2 min; then sequentially carrying out spray water washing and four ultrasonic hot water washing at the temperature of 65 ℃ for 2 min;

a6-4, slow-pull washing, wherein the slow-pull temperature is 85 ℃, the time is 120s, and the conductivity is less than 20 mu m/cm;

a6-5, baking at 75 ℃ for 8 min.

In this embodiment, the vacuum passivation pretreatment mode adopted in step B is a conventional wax and oil removal cleaning treatment, which needs to be matched with ultrasonic waves with an ultrasonic frequency of 40 kHz. Dewaxing at 85 deg.c and pH 9 for 5min, and ultrasonic current 3A; degreasing pH value is 10, temperature is 75 ℃, time is 5 minutes, and ultrasonic current is 3A.

Preferably, an ICP radio frequency passivation process is adopted in the step C, an ICP radio frequency coating process belongs to the optical coating category, the thickness of the film is only a few nanometers, and the coating time in the step C is 10-20 min.

Preferably, the step D adopts an in-furnace AF sealing process, the in-furnace AF belongs to the vacuum evaporation coating category, the coating time is 10-20min, the film thickness is 20-30nm, the main components of the used AF pill are silicon dioxide and perfluoropolyether, and the main components of the AF pill are not greatly different from those of AF fingerprint prevention used in immersion type AF treatment. And D, immediately performing the step C, wherein the furnace door does not need to be opened after the step C is completed, and the workpiece directly and sequentially completes the ICP radio frequency passivation process and the in-furnace AF sealing process in the vacuum coating machine according to a set automatic coating program.

And E, performing neutral salt spray test on the workpiece produced by the process, wherein the workpiece still does not rust after 96 hours of test.

In summary, in the passivation method for the glass and stainless steel packaged workpiece provided by the invention, the overall corrosion resistance of the glass and stainless steel packaged workpiece can be greatly improved by improving the packaging method for manufacturing the stainless steel and the glass into a composite part and combining the passivation technology and the sealing technology to be used for packaging the glass stainless steel assembly, so that the manufactured glass and stainless steel packaged workpiece can be subjected to a neutral salt spray test, and the workpiece still does not rust after 96-hour testing time.

The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.