CN104911535A - Boronizing agent for titanium surface solid boronizing and boronizing process - Google Patents
Boronizing agent for titanium surface solid boronizing and boronizing process Download PDFInfo
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- CN104911535A CN104911535A CN201510362276.9A CN201510362276A CN104911535A CN 104911535 A CN104911535 A CN 104911535A CN 201510362276 A CN201510362276 A CN 201510362276A CN 104911535 A CN104911535 A CN 104911535A
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Abstract
The invention discloses a boronizing agent for titanium surface solid boronizing and a boronizing process. The boronizing agent consists of the following components in percentage by weight: 5 to 93.9 percent of a boron source, 5 to 25 percent of a low-melting-point compound, 1 to 10 percent of a solid oxygen agent and 0.1 to 89 percent of a diluent. During boronizing treatment, the prepared boronizing agent is ball-milled and mixed uniformly and then is put into a boronizing tank, a titanium metal workpiece is buried into the boronizing agent, the temperature is increased to 750-1,300 DEG C, heat preservation is performed for 0.5-24 hours, the workpiece is taken out and cooled by a proper method, and the boronizing agent adhered to the surface of the workpiece is cleaned. The boronizing agent provided by the invention can increase the migration speed from boron to the surface of the workpiece and also can prevent boronizing speed reduction caused by oxidation of a titanium substrate, so that the boronizing efficiency is improved, a thick and uniform permeating layer is easy to obtain, and the boronizing process is safe and environment-friendly.
Description
Technical field
The invention belongs to field of metal surface treatment technology, be specifically related to a kind of titanium surface solid boronising boronizing agent and boriding process.
Background technology
Metal titanium has the advantages such as lightweight, intensity is high, good corrosion resistance, and its metallic substance all has a wide range of applications in many aspects, comprises space flight, military affairs, automobile, medicine equipment, sporting goods, mobile phone etc.But the antiwear property of titanium is poor, oxidizable and suction hydrogen under hot conditions, cause titanium device performance to be deteriorated and even lost efficacy, work-ing life reduces.In recent years, the tribological property of titanium, the research focus that high temperature resistant, corrosion resisting property becomes association area expert is strengthened by titanium surface modification.After the process of titanium surface boronizing, the TiB that surface is formed
2, TiB has higher hardness, good abrasion resistance, good electroconductibility and corrosion resistance nature.Therefore, boronising is a kind of strengthening titanium or titanium alloy material surface performance, improves the good method in its work-ing life.
Pack boriding method technique is simple, and flow process is short.And, during pack boriding method process complex-shaped workpieces, also can obtain the uniform diffusion layer organization of thickness.Therefore, current industrial most popular be pack boriding method, what be most widely used is also this method, and other boronizing methods are generally only stagnated in laboratory study.Traditional pack boriding method is generally carried out in pressed powder, and the B atom produced by boron supplying agent in boronizing agent needs to move to workpiece surface by solid-solid diffusion, and solid-solid diffusion process is extremely slow, and therefore boronising efficiency is lower.Meanwhile, although generally can adopt inert protective atmosphere in boronizing process, under the condition that oxygen partial pressure is lower, some metals (as Ti, Al) also can be oxidized, hinders B to matrix internal diffusion.And, manyly during pack boriding to use KBF
4deng fluoroborate as activator, and fluoroborate can decompose generation BF when boronising
3etc. the gas having toxicity, contaminate environment, threaten operator's personnel safety, and the workpiece of fluorochemical to some material (as Ti) has corrosive nature.In addition, after traditional method boronising, workpiece surface dirt settling difficulty is cleaned out, and this may affect the follow-up use of workpiece.
The present invention is for solving the problem, and propose a kind of titanium surface solid boronising boronizing agent and boriding process, this boronizing agent can provide liquid channel for the diffusion of B in boronizing agent, accelerates the diffusion of B, and workpiece can be protected not oxidized, improves boronising efficiency; This boronizing agent not fluoride, can not produce material environment being had to pollution, and boronizing agent is easily separated with workpiece simultaneously.
Summary of the invention
The object of the invention is to the defect for existing in current pack boriding, provide a kind of boronising efficiency high, boronising workpiece easy to clean, boronizing process is pollution-free, can obtain thickness large and the titanium surface solid boronising boronizing agent of uniform infiltration layer and boriding process.
The object of the invention is to be achieved through the following technical solutions.
A kind of titanium surface solid boronising boronizing agent, boronizing agent is composed of the following components: 5 ~ 93.9wt.% boron source, 5 ~ 25wt.% low melting component, the solid oxygen agent of 1 ~ 10wt.%, 0.1 ~ 89wt.% thinner, wherein boron source comprises one or more in amorphous boron, crystalline boron, ferro-boron, and low melting component comprises B
2o
3, Na
2b
4o
7, Na
2b
2o
4, K
2b
4o
7, K
2b
2o
4, Li
2b
4o
7, K
2cO
3, Na
2cO
3in one or more, Gu oxygen agent comprises one or both in Al powder, Mg powder, thinner comprises Al
2o
3, one or both in MgO.
The preferred proportion scope in boron source is 60 ~ 93wt.%, preferred amorphous boron.
The preferred proportion scope of low melting component is 5 ~ 15wt.%, preferred B
2o
3, Na
2b
4o
7, Na
2b
2o
4, K
2b
4o
7, K
2cO
3, Na
2cO
3in one or more.
Gu the preferred proportion scope of oxygen agent is 1 ~ 6wt.%.
The preferred proportion scope of thinner is 1 ~ 25wt.%.
Use the titanium surface solid boriding process of described boronizing agent,
(1) take each component of boronizing agent by proportioning, mix, for subsequent use;
(2) pre-treatment of titanium workpiece surface, for subsequent use;
(3) boronizing agent after mixing is placed in boronising tank, and by workpiece landfill in boronizing agent, is warmed up to target temperature, insulation, cooling, take out workpiece, the boronizing agent of cleaning workpiece surface attachment.
In step (1), each component of boronizing agent is placed in dry more than the 12h of vacuum drying oven in advance; And adopting ball milling method to mix, Ball-milling Time controls at 2 ~ 18h.
In step (2), the pretreated detailed process of titanium workpiece surface is: use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to surface of workpiece, and removing workpiece surface zone of oxidation also makes surface polish, then workpiece is placed in Ultrasonic Cleaners acetone cleaning 10 ~ 30min, finally clean with deionized water rinsing, dries up, stand-by.
Target temperature in step (3) controls at 750 ~ 1300 DEG C, is preferably 950 ~ 1200 DEG C; Boronising time controling is at 0.5 ~ 24h.
Boronizing agent of the present invention might not be defined in the surface boronizing process of titanium, selects suitable low melting component, solid oxygen agent, also can be used for the Bononizing pretreatment of other metallic substance such as Fe, Ni, Mn, Co.
In boronizing agent of the present invention, the effect of low melting component is to provide liquid phase micro-area, for B provides liquid channel to the migration of workpiece surface, accelerates dissolving and the diffusion of B, improves boronising efficiency.
The binding ability of solid oxygen agent of the present invention and oxygen is better than the binding ability of boron, Ti and oxygen, and this solid oxygen agent is not reacted with Ti matrix.
The effect of thinner of the present invention is the concentration needing boron in Reasonable Regulation And Control boronizing agent according to boronising.
Boronizing agent of the present invention can prevent titanium workpiece surface oxidized in boronizing process, and boronising efficiency is high, and boronizing agent is easily separated with workpiece, and safety, environmental protection, easily obtain the large and uniform titanium base modification boride layer of thickness.The present invention is under preferred boronizing agent component, preferably boronising temperature, preferably boronising time conditions, and can obtain the boride layer that thickness is larger, this can be drawn by the contrast of embodiment 1-5.
Accompanying drawing explanation
Fig. 1 is sample material phase analysis figure in the embodiment of the present invention 1;
Fig. 2 is cross-section morphology figure after sample boronising in the embodiment of the present invention 1.
Embodiment
Be intended to further illustrate the present invention below in conjunction with embodiment, and unrestricted the present invention.
Boriding process step of the present invention is as follows:
(1) preparation of boronizing agent
Each component (being placed in dry more than the 12h of vacuum drying oven in advance) is taken, ball milling mixing 2 ~ more than 18h by proportioning, for subsequent use; (2) pretreatment of metal surface
Use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to titanium workpiece surface, removing surface oxide layer, after workpiece cleaning is clean with deionized water, then workpiece is placed in Ultrasonic Cleaners acetone cleaning 10 ~ 30min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, titanium workpiece landfill is entered boronizing agent, be placed in resistance furnace or electricity stove frequently, pass into rare gas element, be warming up to 750 ~ 1200 DEG C, after insulation 0.5 ~ 24h, titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.The rare gas element adopted comprise in Ar, He one or both.
Embodiment 1
The boronizing agent adopted consists of amorphous boron, Na
2b
4o
7, Al powder, Al
2o
3, concrete proportioning is as shown in table 1.
Table 1 embodiment 1 boronizing agent proportioning raw materials
| Composition | Amorphous boron | Na 2B 4O 7 | Al powder | Al 2O 3 |
| Content (wt.%) | 93 | 5 | 1 | 1 |
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 6h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA1) as boronising workpiece, titanium plate gauge lattice are 40 × 30 × 3mm, use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, then workpiece is placed in Ultrasonic Cleaners acetone and cleans 20min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA1 titanium plate landfill is entered boronizing agent, is placed in resistance furnace, passes into Ar as protective atmosphere, be warming up to 900 DEG C, after insulation 2h, titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
Carry out XRD detection to workpiece, as shown in Figure 1, detected result display workpiece surface infiltration layer is by TiB, TiB for its XRD figure spectrum
2composition.Carry out SEM detection to workpiece interface, its SEM schemes as shown in Figure 2, and can see two-phase boride layer at workpiece surface, skin is TiB
2layer, and thickness is homogeneous, this layer of mean thickness is 4.87 μm, and secondary skin is TiB whisker layer, and this layer crystal mean length must reach 32.87 μm.
Embodiment 2
The boronizing agent adopted consists of amorphous boron, Na
2b
4o
7, Al powder, Al
2o
3, concrete proportioning is as shown in table 2.
Table 2 embodiment 2 boronizing agent proportioning raw materials
| Composition | Amorphous boron | Na 2B 4O 7 | Al powder | Al 2O 3 |
| Content (wt.%) | 93 | 5 | 1 | 1 |
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 6h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA1) as boronising workpiece, titanium plate gauge lattice are 40 × 30 × 3mm, use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, then workpiece is placed in Ultrasonic Cleaners acetone and cleans 20min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA1 titanium plate landfill is entered boronizing agent, is placed in resistance furnace, passes into Ar as protective atmosphere, be warming up to 950 DEG C, after insulation 2h, titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
Carry out XRD detection to workpiece, as shown in Figure 1, collection of illustrative plates display workpiece surface infiltration layer is by TiB, TiB for the XRD figure spectrum of workpiece
2composition, does not find the existence of oxide compound.Carry out SEM detection to workpiece interface, can see two-phase boride layer at workpiece surface, skin is TiB
2layer, and thickness is homogeneous, this layer of mean thickness reaches 6.76 μm, and secondary skin is TiB whisker layer, and this layer crystal mean length must reach 44.78 μm.
Embodiment 3
The boronizing agent adopted consists of amorphous boron, Na
2b
4o
7, Al powder, Al
2o
3, concrete proportioning is as shown in table 3.
Table 3 embodiment 3 proportioning raw materials
| Composition | Amorphous boron | Na 2B 4O 7 | Al powder | Al 2O 3 |
| Content (wt.%) | 65 | 5 | 5 | 25 |
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 6h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA1) as boronising workpiece, titanium plate gauge lattice are 40 × 30 × 3mm, use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, after then workpiece cleaning is clean with deionized water, then workpiece be placed in Ultrasonic Cleaners acetone and clean 20min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA1 titanium plate landfill is entered boronizing agent, is placed in resistance furnace, passes into Ar as protective atmosphere, be warming up to 950 DEG C, after insulation 2h, titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
Carry out XRD detection to workpiece, result display workpiece surface infiltration layer is by TiB, TiB
2composition, does not find the existence of oxide compound.Carry out SEM detection to workpiece interface, can observe two-phase boride layer at workpiece surface, skin is TiB
2layer, and thickness is homogeneous, this layer of mean thickness is 5.19 μm, and secondary skin is TiB whisker layer, and this layer crystal mean length must reach 37.63 μm.
Embodiment 4
The boronizing agent adopted consists of amorphous boron, Na
2b
4o
7, K
2b
4o
7, Mg powder, Al
2o
3, concrete proportioning is as shown in table 4.
Table 4 embodiment 4 proportioning raw materials
| Composition | Amorphous boron | Na 2B 4O 7 | K 2B 4O 7 | Mg powder | Al 2O 3 |
| Content (wt.%) | 60 | 5 | 5 | 5 | 25 |
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 12h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA2) as boronising workpiece, titanium plate gauge lattice are 30 × 30 × 4mm, use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, after then workpiece cleaning is clean with deionized water, then workpiece be placed in Ultrasonic Cleaners acetone and clean 15min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA2 titanium plate landfill is entered boronizing agent, is placed in resistance furnace, passes into Ar as protective atmosphere, be warming up to 1050 DEG C, after insulation 3h, titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
XRD detection is carried out to workpiece, finds can see obvious TiB, TiB in XRD figure spectrum
2characteristic peak, not to find oxide compound.Carry out SEM detection to workpiece interface, can observe two-phase boride layer at workpiece surface, skin is the uniform TiB of thickness
2layer, this layer of mean thickness is 10.51 μm, and secondary skin is the TiB whisker that orientation is consistent, and this layer crystal mean length must reach 49.37 μm.
Embodiment 5
The boronizing agent adopted consists of amorphous boron, crystallization boron, Na
2b
4o
7, K
2b
4o
7, Na
2cO
3, Mg powder, MgO, concrete proportioning is as shown in table 5.
Table 5 embodiment 5 proportioning raw materials
| Composition | Amorphous boron | Crystallization boron | Na 2B 4O 7 | K 2B 4O 7 | Na 2CO 3 | Mg powder | MgO |
| Content (wt.%) | 40 | 20 | 10 | 10 | 5 | 5 | 10 |
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 8h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA1) as boronising workpiece, titanium board size specification is 30 × 30 × 4mm, uses 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, after then workpiece cleaning is clean with deionized water, then workpiece be placed in Ultrasonic Cleaners acetone and clean 20min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA2 titanium plate landfill is entered boronizing agent, is placed in resistance furnace; the mixed gas passing into He and Ar, as protective atmosphere, is warming up to 1050 DEG C, after insulation 3h; titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
XRD detection is carried out to workpiece, only TiB, TiB detected
2existence.SEM detection is carried out to workpiece interface, two-phase boride layer can be observed at workpiece surface, TiB
2layer thickness is 8.74 μm, and TiB whisker mean length is 38.94 μm.
Comparative example 1
Adopt the boronising of conventional solid boronizing agent, contrast with the present invention, boronizing agent consists of 65wt.%B
4c, 35wt.%KBF
4.
(1) preparation of boronizing agent
Take each component after above-mentioned oven dry respectively by proportioning, ball milling 6h, mixes, for subsequent use.
(2) pretreatment of metal surface
Select titanium plate (TA2) as boronising workpiece, titanium board size specification is 30 × 30 × 4mm, uses 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to workpiece, removing surface oxide layer, after then workpiece cleaning is clean with deionized water, then workpiece be placed in Ultrasonic Cleaners acetone and clean 20min, finally clean with deionized water rinsing, dries up, stand-by;
(3) Bononizing pretreatment
The boronizing agent prepared is loaded boronising tank, meanwhile, TA2 titanium plate landfill is entered boronizing agent, is placed in resistance furnace; the mixed gas passing into He and Ar, as protective atmosphere, is warming up to 1050 DEG C, after insulation 3h; titanium workpiece is taken out, cools in a suitable manner, the ionogen of cleaning attachment.
XRD detection is carried out to workpiece, can TiB, TiB be detected
2existence.SEM detection is carried out to workpiece interface, two-phase boride layer can be observed at workpiece surface, but boride layer thickness is less, TiB
2layer thickness is only 4.5 μm, and TiB whisker mean length is only 23 μm, and infiltration layer total thickness is 27.5 μm, far below the alloying layer thickness obtained under temperature same in the embodiment of the present invention 4, time conditions.
Claims (10)
1. a titanium surface solid boronising boronizing agent, it is characterized in that, boronizing agent is composed of the following components: 5 ~ 93.9wt.% boron source, 5 ~ 25wt.% low melting component, the solid oxygen agent of 1 ~ 10wt.%, 0.1 ~ 89wt.% thinner, wherein boron source comprises one or more in amorphous boron, crystalline boron, ferro-boron, and low melting component comprises B
2o
3, Na
2b
4o
7, Na
2b
2o
4, K
2b
4o
7, K
2b
2o
4, Li
2b
4o
7, K
2cO
3, Na
2cO
3in one or more, Gu oxygen agent comprises one or both in Al powder, Mg powder, thinner comprises Al
2o
3, one or both in MgO.
2. titanium surface solid boronising boronizing agent according to claim 1, is characterized in that, the preferred proportion scope in boron source is 60 ~ 93wt.%, preferred amorphous boron.
3. titanium surface solid boronising boronizing agent according to claim 1, is characterized in that, the preferred proportion scope of low melting component is 5 ~ 15wt.%, preferred B
2o
3, Na
2b
4o
7, Na
2b
2o
4, K
2b
4o
7, K
2cO
3, Na
2cO
3in one or more.
4. titanium surface solid boronising boronizing agent according to claim 1, is characterized in that, Gu the preferred proportion scope of oxygen agent is 1 ~ 6wt.%.
5. titanium surface solid boronising boronizing agent according to claim 1, is characterized in that, the preferred proportion scope of thinner is 1 ~ 25wt.%.
6. use the titanium surface solid boriding process of the boronizing agent described in any one of claim 1-5, it is characterized in that,
(1) take each component of boronizing agent by proportioning, mix, for subsequent use;
(2) pre-treatment of titanium workpiece surface, for subsequent use;
(3) boronizing agent after mixing is placed in boronising tank, and by workpiece landfill in boronizing agent, is warmed up to target temperature, insulation, cooling, take out workpiece, the boronizing agent of cleaning workpiece surface attachment.
7. titanium surface solid boriding process according to claim 6, is characterized in that, in step (1), each component of boronizing agent is placed in dry more than the 12h of vacuum drying oven in advance; And adopting ball milling method to mix, Ball-milling Time controls at 2 ~ 18h.
8. titanium surface solid boriding process according to claim 6, is characterized in that, in step (2), the pretreated detailed process of titanium workpiece surface is: use 180 successively
#, 400
#, 600
#, 800
#, 1000
#, 1200
#abrasive paper for metallograph carries out mechanical polishing process to surface of workpiece, and removing workpiece surface zone of oxidation also makes surface polish, then workpiece is placed in Ultrasonic Cleaners acetone cleaning 10 ~ 30min, finally clean with deionized water rinsing, dries up, stand-by.
9. titanium surface solid boriding process according to claim 6, is characterized in that, the target temperature in step (3) controls at 750 ~ 1300 DEG C, is preferably 950 ~ 1200 DEG C; Boronising time controling is at 0.5 ~ 24h.
10. the application method of the titanium surface solid boronising boronizing agent described in any one of claim 1-5, is characterized in that, can be used for the Bononizing pretreatment of the metallic substance comprising Fe, Ni, Mn, Co.
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109182961A (en) * | 2018-10-29 | 2019-01-11 | 山东建筑大学 | A kind of workpiece surface reinforcing low-temperature solid B-Cr-Re reducing agent |
| CN114836711A (en) * | 2022-05-10 | 2022-08-02 | 长沙特耐金属材料科技有限公司 | Metal surface hardening method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109182961A (en) * | 2018-10-29 | 2019-01-11 | 山东建筑大学 | A kind of workpiece surface reinforcing low-temperature solid B-Cr-Re reducing agent |
| CN114836711A (en) * | 2022-05-10 | 2022-08-02 | 长沙特耐金属材料科技有限公司 | Metal surface hardening method |
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| Publication number | Publication date |
|---|---|
| CN104911535B (en) | 2017-06-09 |
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