Journal Pre-proof

Study of Fracturing Fluid on Gel Breaking Performance and Damage to fracture

conductivity

Jie Wang, Yixiao Huang, Yan Zhang, Fujian Zhou, Erdong Yao, Rui Wang

PII: S0920-4105(20)30514-3
DOI: https://doi.org/10.1016/j.petrol.2020.107443
Reference: PETROL 107443

To appear in: Journal of Petroleum Science and Engineering

Received Date: 17 November 2019

Revised Date: 18 May 2020
Accepted Date: 19 May 2020

Please cite this article as: Wang, J., Huang, Y., Zhang, Y., Zhou, F., Yao, E., Wang, R., Study of
Fracturing Fluid on Gel Breaking Performance and Damage to fracture conductivity, Journal of
Petroleum Science and Engineering (2020), doi: https://doi.org/10.1016/j.petrol.2020.107443.

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 Credit Author Statement
Manuscript title: Study of Fracturing Fluid on Gel Breaking Performance and Damage to Fracture
Conductivity

All data in the article comes from the author, without plagiarism and copyright issues.

Author signature: Jie Wang,Yixiao Huang, Yan Zhang, Fujian Zhou, Erdong Yao, Rui Wang
Date: 14th-04-2020.
 1 Study of Fracturing Fluid on Gel Breaking Performance and Damage to
2 Fracture Conductivity
3 Jie Wang a,b, Yixiao Huang a,b, Yan Zhangc, Fujian Zhoua,b,*, Erdong Yaoa,b, Rui Wangd
a
4 Unconventional Natural Gas Institute, China University of Petroleum at Beijing, 102249, China
b
5 State Key Laboratory of Petroleum Resource and Prospecting, China University of Petroleum at
6 Beijing, 102249, China
c
7 Gudao Oil Picking Factory, Shengli Oilfield, Sinopec, 257000, China
d
8 Schlumberger China, 100015, China
9 *Corresponding Author: zhoufj@cup.edu.cn
10 Abstract: As a thickening agent commonly used in hydraulic fracturing, guar gum has the
11 advantage of low price and excellent performance. However, the gel breaking mechanism of
12 fracturing fluid under high temperature and high pressure environment and the damage
13 mechanism to the reservoir needs further study. The current criteria for judging gel breaking is
14 based on the viscosity of the solution being less than 5 mPa.s, however it’s not always true that the
15 gel breaks even if the viscosity of the fluid is low. To solve this problem, it’s recommended in this
16 paper to analyze the gel breaking performance of fracturing fluid by measuring the median
17 molecular particle size and the residue content together with the viscosity of fracturing fluid.
18 Moreover, the effects of the gel breaker on the crushing and formation embedding of the proppant,
19 the adsorption and retention mechanism of the residue in the induced fracture and their influence
20 on the conductivity are investigated. Studies show that the gel breaking performance of guar gum
21 fracturing fluid is affected by the amount of gel breaker and temperature. Adding extra amount of
22 gel breaker and imposing high temperatures do not effectively reduce the median molecular
23 particle size of the fracturing fluid. The detrimental effect of the gel breaker and it’s residue to the
24 fracture conductivity is mainly reflected in three aspects: increased crush rate of the proppant due
25 to soaking in the gel breaker, exacerbated embedding of the proppant into formation due to
26 interaction of the fluid and the formation and the reduced pore diameter of the formation due to
27 residue of the fracturing fluid. It’s observed that the detrimental effect of the gel breaker on the
28 conductivity of the fracture is mostly in the area with a high closing pressure of 50 MPa or above.
29 This study provides a reference of tight sandstone reservoirs hydraulic stimulation and fracturing
30 fluid formation damage for high temperature and high pressure oilfields like Tarim oilfield.
31 Keywords: Gel breaking of fracturing fluid; Fracturing fluid residue; Proppant crush; Proppant
32 embedding; Conductivity
33 1 Introduction
34 For ultra-deep high-temperature unconventional oil/gas reservoirs, hydraulic stimulation is a
35 common method of increasing production. Guar gum is a natural vegetable gum with excellent
36 performance. It is widely used as a thickening agent in hydraulic fracturing. The fracturing fluid
37 used on operation must have good sand-carrying performance, easy to break gel at the reservoir
38 temperature and low damage of residue, etc. (Qiu et al., 2018a; Qiu et al., 2018b; Sun et al., 2019;
39 Zhang et al., 2018; Zhang et al., 2019a). However, since the guar gum itself contains insoluble
40 residue such as protein, coarse fiber, large molecular weight galactomannan, and ash, etc., the
41 fracturing fluid breaks gel incompletely and a large amount of insoluble residue produced in the
42 gel breaking process blocks the passage and thereby compromising the result of hydraulic
43 stimulation (Ihejirika et al., 2015; Kolb, 1971). The research on formation damage of guar gum
44 fracturing fluid’s has been more than 60 years (Allen and Hough, 1957). In 1979, the mechanism
45 of fracturing fluid damage to reservoir was revealed that capillary pressure and relative
46 permeability are two important factors affecting the flowback of fracturing fluid (Holditch, 1979;
47 Thomas et al; 2019). The degree of damage on the fracture surface is related to the intrusion depth
48 of the fracturing fluid and the skin effect (Volk et al., 1983). During the multi-stage fracturing
49 process of horizontal wells, fracturing fluid also do damage to the reservoir (Aymen et al., 2018;
50 Yu and Guo, 2010; Zhao et al., 2019). Quantitative analysis results show that the fracturing fluid
51 can cause damage to shale, mudstone and tight carbonate rocks (Pagels et al., 2013). At the same
52 time, the damage of hydroxypropyl guar fracturing fluid to natural fractures from sandstone in
53 different regions (Gall et al., 1988; Wu et al., 2019; Zhang et al, 2018). The novel unsteady
54 method can quickly study the water sensitivity, water locking and solid particle damage of
55 fracturing fluid (Zhang et al., 2019b).. However, the above studies all focused on the damage of
56 fracturing fluid to reservoir permeability or natural fracture, but rarely considered the influence of
57 fracturing fluid inside the incuded propped fracture. Weaver et al. studied the damage of fracture
58 conductivity by drilling fluid and fracturing fluid through a rapid colloid damage evaluation
59 method (Weaver et al., 2013). Yang et al. studied the effect of fracturing fluid retention on fracture
60 conductivity in shale and conventional oil and gas reservoirs (Zhao et al., 2018; Yang et al., 2017).
61 Wu et al. eliminated the experimental errors of using different cores through the improvement of
62 experimental methods and evaluated the influence of different types of fracturing fluids on the
63 fracture conductivity of shale cores (Hu et al., 2018; Sun et al., 2018; Wu et al., 2017). All the
64 above studies on the damage of the fracture conductivity by various factors in a macroscopic
65 perspective did not conduct in-depth research on the mechanism/cause of the damage. Therefore,
66 it is necessary to research on the microscopic mechanism of fracturing fluid damage to the
67 propped fracture.
68 It is generally conceived that the detrimental effect of fracturing fluid on the conductivity mainly
69 comes from the following two aspects: 1) The interaction between fracturing fluid and rock causes
70 changes in the physical and mechanical properties of the rock, increasing the embedding of the
71 proppant. 2) The retention of fracturing fluid residue in the fracture and on the surface of the
72 proppant reduces conductivity of the propped fracture. Zhang et al. believe that fluid/rock
73 interaction may lead to a significant decrease in Young’s modulus of the rock therefore enhancing
74 proppant embedding. At the same time, due to the increased depth of proppant embedding, the
75 pore size of the fracture is reduced thus both fracture conductivity and production efficiency are
76 greatly affected (Zhang et al., 2015a&b&2017; Zhong et al., 2019). However, it’s neglected that
77 the effect of proppant crush and that the crush rate becomes more severe at high formation closing
78 pressure and soaking of the fracturing fluid. Whether the fracturing fluid affects the crush rate of
 79 the proppant needs to be considered and studied simultaneously. Singh et al., believe that the type
80 and concentration of metal ions in the fracturing fluid increases the residue content, which in turn
81 affects the fracture conductivity (Singh et al., 2015; Beckwith, 2012). Huang et al. found that
82 fracturing fluid residue is more harmful to stimulated fracture than natural fracture (Huang and
83 Liu, 2019; Li and Misra, 2018; Wu et al., 2018). However, the microscopic adsorption of residues
84 in the fracture has not been studied in depth.
85 The damage of the fracturing fluid to the fracture conductivity is closely related to the gel
86 breaking performance of the fracturing fluid, and the fracturing performance of the fracturing fluid
87 is strongly controlled by the temperature and the amount of the gel breaker. In this paper, the study
88 the effect of gel breaker’s concentration and temperature on the gel breaking performance of
89 fracturing fluid is firstly presented, and the investigation on the effect of gel breaking fracturing
90 fluid and residue on fracture conductivity by macroscopic conductivity test and microscopic
91 scanning experiments are detailed. This study provides reference for Tarim oilfield, fracture
92 operation in other high-temperature and high-pressure tight sandstone reservoirs and fracturing
93 fluid damage study.
94 2 Laboratory Study
95 2.1 Test Material
96 Fluid tested: fracturing fluid composition: 0.5 wt% Hydroxypropyl guar gum (JK101) + 1 wt%
97 stabilizer (KWD-105H) + 1 wt% cleanup additive (HSC-25) + 1 wt% clay stabilizer (AS-55) +
98 0.85 wt% conditioning agent (YC-150) + 0.55 wt% cross-linkerx(YP-150). The mix water was
99 distilled water, and the gel breaker was ammonium persulfate, which was taken from the field. The
100 formation water is simulated with 2 wt% KCl solution. High-temperature shear test was carried
101 out on the concentration of 0.3 wt%, 0.4 wt% and 0.5 wt% guar fracturing fluid. The test results
102 are shown in Figure 1(A). When the temperature reaches 155 ℃, the viscosity of 0.5 wt% guar
103 fracturing fluid is still greater than 150 mPa•s, and the performance of the fracturing fluid at that
104 concentration meets the requirements of high temperature fracturing. Collect the the supernatant
105 after the gel broken fracturing fluid was centrifuged at 3000 r/min for 30 mins. Figure 1(B) shows
106 the results of the viscoelasticity test of the cross-linked guar fracturing fluid. The viscosity
107 modulus of the fluid increases with the increase of the scanning frequency, and the elastic modulus
108 decreases with the increase of the scanning frequency.
 (B) 0.5 wt% Guar fracturing fluid viscoelastic
(A) Shear resistance test of guar fracturing fluid
test results
Figure 1. Guar fracturing fluid rheological Properties
109 Notes: 0.5 wt% Guar fracturing fluid recipe: 0.5 wt% Hydroxypropyl guar gum (JK101) + 1 wt%
110 stabilizer (KWD-105H) + 1 wt% cleanup additive (HSC-25) + 1 wt% clay stabilizer (AS-55) +
111 0.85 wt% conditioning agent (YC-150) + 0.55 wt% cross-linkerx(YP-150)
112 Proppant: The proppant used in this study was 30/50 mesh Carbo-HSP proppant, produced by the
113 U.S. company CARBO, and the main component of the proppant is bauxite.. The proppant was
114 soaked in 2 hrs and 24 hrs separately in the breaker, and then dried at 120 for 12 hrsto study the
115 effect of the breaker on the proppant.
116 Rock Slab: The rock slab of formation was taken from the Keshen gas field in the Tarim Basin,
117 Western China. The gas reservoir is buried more than 7000 m deep with 120 °C~160 °C formation
118 temperature, and the average permeability is less than 0.09 mD. It is a typical high-temperature
119 and high-pressure natural fracture type tight sandstone gas reservoir. The formation sample was
120 processed into standard rock plates according to API RP56/58/60 standard, and the surface of the
121 rock sample was polished to eliminate the influence of the roughness on the experimental results
122 (API Recommended Practice 56, 1995; API Recommended Practice 58, 1995; API Recommended
123 Practice 60, 1995). The size of the rock slab is: length 17.74 cm ± 0.04 cm, width 3.76 cm ± 0.05
124 cm, thickness greater than 0.90 cm and less than 2.80 cm, both ends of the rock slab are
125 arc-shaped, and the matrix permeability is 0.035 mD. A steel plate of same size was used for
126 parallel comparison of the embedding test to understand the damage caused by the proppant
127 embedding in the rock.
128 Laboratory Apparatus: 101 type electric thermostatic drying oven (Shanghai Ke Heng Industrial
129 Co., Ltd), UbbeloHde Viscometer (Shanghai Glass Instrument Factory One), laser particle size
130 tester (Zhuhai Omec Instrument Co., Ltd), high precision balance (Sartorius Mechatronics(Beijing)
131 Co., Ltd), high speed centrifuge (Hunan Xiang Yi Laboratory instrument development Co., Ltd),
132 oil bath pan (Taicang Experimental Equipment Factory), FCS-842 conductivity tester (U.S.
133 company Core Lab). ST-400 three-dimensional shape scanner (NANOVEA), whose vertical
134 measurement range was 27 mm, automatic scanning range in XY direction was 150*150 mm,
135 minimum scan step size was 0.1 μm, scanning speed was 20 mm/s; ultra-high resolution field
136 emission scanning electron microscope (German company Karl Zeiss), whose minimum
137 resolution was 0.8 nm @ 15 kV, magnification was 12-2,000,000 times.
138 2.2 Experiment
139 2.2.1 Fracturing Fluid Gel Breaking Experiment
140 Take the intermediate formation temperature of 140 to determine the optimum amount of
141 breaker. Add different concentrations of breaker to the prepared guar gum fracturing fluid, then
142 pour into sealed iron container and pressurize to 5 MPa and placed in oil bath of various
143 temperatures to investigate temperature effect. The detail experiment scheme is shown in Table 1.
144 During the test, the viscosity of the fracturing fluid was measured at different time intervals in the
145 oil bath. To ensure the accuracy of the experimental results, test was done for six times and results
146 was averaged.
147
148 Table 1. Experiment scheme of the influence of gel breaking agent and temperature on the gel
149 breaking performance
Experiment 1. Under constant temperature (140 )
300 ppm 400 ppm 500 ppm 600 ppm
Experiment 2. Under constant gel breaker concentration (400 ppm)
120 130 140 150 160
150 2.2.2 Testing of the Fluid Median particle size
151 In this study, Top-Sizer laser particle size analyzer was used to analyze the particles and the size of
152 the residue in the broken fluid. The device can measure dispersed samples in liquids, as well as
153 powder samples dispersed in gas, with a molecular size ranging from 0.02 μm to 20,000 μm. The
154 measurement steps as following:
155 (1) Set the ultrasonic time (10 mins) and circulation speed (2000 r/min) in the operation interface,
156 and press the circulation and water inlet keys. After the water is full, press the outlet key to clean
157 the circulation pool, repeat the above steps three times;
158 (2) Click the calibration in the test window to achieve the best light path. The test can only be
159 performed when the reference value is less than 10;
160 (3) Pour 100 ml of the sample to be tested into the circulation pool until the shading rate exceeds
161 50, turn on the ultrasonic wave, adjust the power to 100 W, and shake for 10 mins to make the
162 guar molecules fully and evenly distributed;
163 (4) Create a test file, click "General Test", open the cycle system, the cycle speed is 2000 r/min,
164 then click continuous measurement, start particle size measurement, record the data, click Save;
165 (5) Repeat the above steps three times, record and analyze the measured experimental data,
166 remove the error values, and take the average value to ensure the accuracy of the results.
167 2.2.3 Fracture Conductivity Test and Microscopic Damage Test
168 The test procedure is as follows as shown in Table 2: (1) Install the lower piston and the lower
169 rock plate (or steel plate); (2) Apply a layer of silica gel on the side of the rock plate to fill the
170 clearance between the rock plate and the diversion chamber to prevent fluid leakage; (3) Spread
171 30/50 mesh Carbo-HSP proppant evenly on the surface of the rock plate or steel plate with 4
172 kg/m2 sand loading, which is the same loading used in the field; (4) Install the upper rock plate
173 (or steel plate) and the upper piston, apply5 MPa closing pressure, then inject different fluids into
174 the flow chamber, and ramp the temperature to 140 °C (5) Apply different closing pressures and
175 calculate the conductivity; (6) SEM imaging, EDX elemental analysis techniques were utilized to
176 observe the changes of the proppant micro-morphology before and after the experiment, and the
177 surface residue components of the proppant, hence the microscopic damage to proppant by the
178 breaker is assessed (The sample provided by us and was tested by the State Key Laboratory of
179 China University of Petroleum); (7) 3D morphological scanning experiment was used to study the
180 difference in embedding extent of rock surface from different fluids. The main equipment and
181 process of the experiment are shown in Figures 2-3.
182 Table 2. Experimental scheme of conductivity tests
Flow Rate
NO Sample Injected fluids Temperature Proppant
ml/min
Simulated
Test 1 Steel plate 140 5.00 No treatment
formation water
Simulated Soak in gel breaking
Test 2 Steel plate 140 5.00
formation water liquid for 2 hrs
Simulated Soak in gel breaking
Test 3 Steel plate 140 5.00
formation water liquid for 24 hrs
Simulated
Test 4 Rock slab 140 5.00 No treatment
formation water
Non-residue
Test 5 Rock slab 140 5.00 No treatment
fracturing fluid
Gel breaking for
Test 6 Steel plate 140 5.00 No treatment
60 mins

183
184 Figure 2. Preparation of Core Sample

185
186 Figure 3. Flow chart of flow conductivity and micromorphology test
187 3 Experimental results and discussion
188 3.1 Effect of the amount of breaker on the gel breaking process at high temperature
189 3.1.1 Effect of the amount of breaker on the time of breaking
190 For a specific fracturing fluid system, it is necessary to determine the optimum amount of breaker
191 at a particular temperature. The intermediate value of the selected temperature range was 140 ℃
192 as the reference point. Different concentration of the breaker (300 ppm, 400 ppm, 500 ppm, 600
193 ppm) was added to the guar gum fracturing fluid to study the variation of the breaking time of the
194 fracturing fluid. Figure 4 is a graph showing the relationship between the breaking time of the
195 fracturing fluid at 140 ℃ and different amount of breaker. The result shows that when the
196 amount of breaker is increased from 300 ppm to 400 ppm, the reduction of time to break the gel is
197 48.00%. Wheras as the amount of the breaker is furtherly increased, the time to break the gel tends
198 to be flat. When the breaker concentration is lower than 400 ppm, the polymer molecular chain
199 breakage rate is slower; when the breaker concentration is more than 400 ppm, most polymer
200 molecular chains have been broken, and increasing the concentration of the breaker does not
201 significantly change the breaking speed (Hakiki et al., 2015). From cost point of view, the
202 optimum amount of breaker concentration is 400 ppm. Under this concentration, the fracturing
203 fluid breaks fast, ensuring that the fracturing fluid breaking in time, therefore minimize formation
204 damage.
205

206
207 Figure 4. The influence of the amount of gel breaker on gel breaking time
208 3.1.2 Effect of the amount of gel breaker on the median particle size of broken fracturing
209 fluid
210 From the above experimental, it’s concluded that the increase of the amount of the breaker could
211 effectively reduce the gel breaking time of the fracturing fluid. But whether the gel breaker could
212 effectively reduce the molecular size of the polymer is also one of factors need to be evaluated.
213 The effect of the amount of breaker on the molecular size of the guar gum at 140 °C was tested
214 using a laser particle size analyzer (Figure 5). As the oil bath curing time increased, the median
215 diameter of the fracturing fluid gradually decreased from 137 μm to 95-112 μm. While under the
216 same heating time, the greater the concentration of the breaker, the lower the median diameter of
217 molecular size after gel breaking. When the concentration of the breaker was more than 400 ppm,
218 the median diameter reduction tended to flat out, and when the concentration of breaker was at
219 400 ppm to 600 ppm, the median diameter tended to remain consistent.
220
221 Figure 5. The influence of the amount of gel breaking agent on molecular size of gel breaking
222 liquid
223 3.1.3 Effect of the amount of gel breaker on the amount of residue
224 The weight and structure change of guar molecular during gel breaking affects the solubility of the
225 guar gum and is directly related to conductivity reduction in the propped fracture. Many studies
226 had shown that the solubility of guar gum molecules was mainly related to the ratio of galactose
227 (G) to mannose (M) and the distribution of galactose in the molecular chain. At 140 °C, the
228 residue content of the gel broken solution after adding different concentrations of the breaker was
229 tested, and the relationship between the amount of the residue of the fracturing fluid and the
230 heating time after breaking the gel was plotted. The content of the guar residue was calculated
231 according to the following formula (McDonald, 2005; Burke and Park, 2000):

232 η = m 3 V0 ×1000 (1)

233 In the formula: η-breaking residue content, ppm; m3-residue content, mg; V0-breaking amount, ml.
234 As shown in Figure 6, the longer the heating time and the greater the concentration of the breaker
235 was, the higher the residue content in the breaker. This is mainly because the increase in the
236 amount of the gel breaker accelerated the cleavage of the side chain of the guar gum molecule.
237 When the amount of the low molecular guar gum in the solution reached the solubility upper limit,
238 the residue content increased. The increase heating time would also produce more insolubles and
239 increase the amount of residue (Yu and Guo, 2010). For field application, the optimum
240 concentration of the breaker is 400 ppm.
241
242 Figure 6. The influence of the amount of gel breaker on the amount of residue
243 3.2 Effect of Temperature on Performance of Gel Breaking Fracturing Fluid
244 Based on the above study, it is determined that the optimal amount of the gel breaker is 400 ppm.
245 The effects of temperature on the time of gel breaking of the fracturing fluid, the median
246 molecular size of the gel breaker and the residue content were studied separately.
247 3.2.1 Effect of Temperature on Time of Gel Breaking of Fracturing Fluid
248 Although the reservoir temperature in the Keshen area was up to 160 °C, the pre-flush would
249 significantly cool down the formation during the fracturing operation. Therefore, it was necessary
250 to study the gel breaking time of the fracturing fluid at different temperatures. In general, when the
251 viscosity of the fracturing fluid was less than 5 mPa·s, it is considered to be completely broken
252 with the viscosity before breaking as high as 900 mPa·s. Figure 7 shows the relationship between
253 the logarithm of the viscosity of the fracturing fluid at different temperatures and the heating time
254 at 400 ppm breaker concentration, and Figure 8 was the time to break the gel at different
255 temperatures at 400 ppm breaker concentration. The corresponding gel breaking times of 120 °C,
256 130 °C, 140 °C, 150 °C and 160 °C were 25 mins, 20 mins, 15 mins, 12.5 mins, and 10 mins,
257 respectively. These indicates that the higher the temperature is, the faster the fracturing fluid
258 breaks. The results showed that the fracturing fluid could break the gel quickly at different
259 temperatures and achieve quick flowback.

Figure 7. The influence of temperature on gel Figure 8. Guar gum fracturing fluid breaking
breaking time, breaker concentration = 400 ppm time at different temperatures, breaker
concentration = 400 ppm
260 3.2.2 Effect of Temperature on the Median Diameter of Molecular Size of Gel Breaker
261 According to the above study, the viscosity changed greatly before and after breaking the gel, but
262 the final gel viscosity was almost the same. According to Mark-Houwink’s empirical formula (He
263 et al., 2007; Guo and He., 2012), it could be seen that the viscosity of the fracturing fluid is
264 exponentially related to the molecular weight. Therefore the gel breaking performance of the
265 fracturing fluid cannot be fully characterized by viscosity. Hence the median particle size method
266 was introduced. The method was used to further investigate the gel breaking properties.
267 The laser particle size test was carried out on the gel breaker of different heating time before and
268 after the gel breaking. The results were shown in Figure 9. After the gel breaking, the median
269 diameter of the fracturing fluid changed greatly while the viscosity of the fracturing fluid fallen
270 sharply simultaneously. The median diameter reduction slowed down beyond this point. The final
271 result shows that the median particle size of the fracturing fluid reduced from 137 μm before gel
272 breaking to 90 μm after gel breaking, and the range of change was between 28.47% and 36.50%. It
273 could be seen from 3.2.1 that the viscosity of the fracturing fluid reduced from 900 mPa·s to less
274 than 5 mPa·s with the range of change more than 99%. Therefore, as the heating time increased,
275 the viscosity reduction was much more than the median diameter reduction, indicating there are
276 still larger size molecules in the solution after the fracturing fluid broke. These larger size guar
277 gum molecules precipitates to form a residue, that was, reduces the fracturing fluid flowback rate,
278 and at the same time reduced the fracture conductivity due to bridging effect.

279
280 Figure 9. Relation between median molecular particle size of guar gum molecule and heating time
281 at different temperatures, breaker concentration = 400 ppm
282 3.2.3 Effect of Temperature on the Residue Content of Gel Breaker
283 The median particle size of the fracturing fluid was still about 90 μm after breaking and heating,
284 which would affect the content of the residue. Fracturing fluid residue could also cause certain
285 damage to the reservoir, so it was necessary to determine the effect of temperature on the residue
286 content. Figure 10 shows the relationship between the residue content and the heating time at
287 different temperatures. It could be seen that with the increase of heating time, the content of
288 fracturing fluid residue at different temperatures gradually increased. The reason behind is as the
289 bath time increases, the precipitation worsening and residue content increases. The higher the
290 temperature, the faster the molecular chain of guar broke and the more insoluble matter was
291 produced. Therefore, the residue content in the high temperature environment was higher under
292 the same heating time. From molecular structure perspective, in the initial stage of oxidation gel
293 breaking, the destruction of the side chain galactose bond would cause a significant decrease in the
294 solubility of guar gum molecules (McDonald, 2005; Burke and Park, 2000), and some guar
295 molecules separated out from the solution and formed flocculent precipitate. Therefore, the
296 increase of temperature and heating time accelerated the destruction rate of the side chain
297 galactose bond and increased the residue content of the gel breaker.

298
299 Figure 10. Relationship between fracturing fluid residue content and heating time at different
300 temperatures, breaker concentration = 400 ppm
301 3.3 Damage to the Conductivity of Propped fracture by Gel Breaker
302 It could be seen from the above studies that the amount of breaker and temperature had a certain
303 influence on the gel breaking performance of the fracturing fluid. Excessive gelling agent and
304 higher temperature would increase the residue content of the gelling solution. The factors which
305 effect the conductivity include compromised proppant strength due to physicochemical action
306 from broken gel fluid soaking, the degree of embedding of the proppant into the formation rock,
307 and the retention of the residue formed by the gel breaker (Raysoni and Weaver, 2012; Weaver and
308 Raysoni, 2010). Therefore, the following three aspects were studied for the effect of the gel
309 breaking liquid on the crush rate of the proppant, the degree of embedding and the influence of the
310 fracturing fluid residue on the conductivity of the propped fracture.
311 3.3.1 Study on the Damage of the Conductivity Caused by the Crush and Embedding of the
312 Proppant
313 (1) Study on the damage of the conductivity caused by the crush of proppant
314 In order to study the effect of the remaining gel breaking liquid on the proppant performance,
315 under 140 °C the proppant was soaked in the broken fluid for 2 hrs and 24 hrs separately and
316 compared with proppant without soaking. After drying, the crush rate was measured under the API
317 standard. The result was shown in Figure 11. It could be seen that as the closing pressure increases,
318 the proppant crush rate under all three conditions increased continuously. When the closing
319 pressure was lower than 40 MPa, the three proppant crush rates had little difference; when the
320 closing pressure was higher than 40 MPa, the three proppant crush rates were significantly
321 different, and the proppant crush rate of the soaked over-gelling agent was higher than that. Soak
322 the proppant of the gel breaking liquid, and the higher the pressure, the longer the soaking time
323 was and the greater the fracture rate of the proppant was. This was mainly due to the occurrence of
324 rock/fluid reaction of the proppant under the immersion of high temperature gel breaking liquid,
325 destroying the structure and strength of the proppant on the contact surface, making the proppant
326 brittle under the action of the closing pressure (Weaver and Raysoni, 2010).

327
328 Figure 11. The change in proppant crush rate caused by gel breaking solution (Heating
329 temperature = 140 °C, breaker concentration = 400 ppm)
330 In order to study the degree of damage to the conductivity of the proppant after crushing, take the
331 proppant without soaking the gel breaking fluid, soaking 2 hrs, soaking 24 hrs, and testing the
332 conductivity with distilled water at 140 (Test 1, Test 2, Test 3). The proppant conductivity value
333 (Test 2, Test 3) after soaking was compared with the unsoaked proppant conductivity value (Test
334 1), and the change value was used as the damage rate. The experimental result was shown in
335 Figure 12. It could be seen that as the closing pressure increases, the damage rate of the soaking
336 gel breaking fluid to the conductivity was gradually increased from 1.4% to about 20%. Under
337 low closure stress, the proppant break rate was lower, and the damage rate of the conductivity was
338 also lower. The longer the soaking time was, the higher the damage rate was at the same closing
339 pressure.
340
341 Figure 12. Proppant conductivity after soaking in fracturing fluid
342 (2) Damage to the conductivity caused by gel breaking fluid intensifying proppant crush and
343 embedding
344 In order to study the degree of damage caused by proppant crush and embedding, the rock
345 conductivity experiment was carried out (Test 4: Slab-formation water conductivity experiment,
346 Test 5: Slab - Filtration of the broken liquid conductivity experiment). A comparison test of steel
347 plate was ran (Test 1) to calculate the rate of damage of the conductivity. In the experiment, the
348 formation water and the filtration of gel breaking fluid were selected to compare whether the fluid
349 reacted with the rock in high temperature environment and whether the proppant was broken and
350 embedded. The gel breaking fluid was filtered to eliminate the residue’s damage to propped
351 fracture. As shown in Figure 13, it could be seen that, under 50 MPa, the conductivity of the three
352 was not much different, the proppant was broken and embedded at a low pressure, and the
353 influence of the breaker on the proppant was negligible. When the closing pressure was 50 MPa,
354 the rock conductivity and the damage rate both had turning points, indicating that the proppant
355 crushing and embedding mainly occurred when the closing stress was greater than 50 MPa. The
356 damage rate of the slab-filtering gel breaking fluid experiment was higher than that of the
357 slab-formation water, indicating that the potential reaction of fluid/rock slab intensifies the
358 embedding of the proppant in the high temperature environment.
359
360 Figure 13. The influence of proppant embedding on conductivity induced by fracturing fluid
361 In order to further verify whether the gel-breaking fluid would intensify the embedding of the
362 proppant, the surface morphology of the rock samples after the test of the Test 4 and Test 5 rock
363 plates was scanned and characterized using a three-dimensional shape scanner to study the
364 difference of proppant embedding, which caused by the fluid/rock reaction. Formation water was
365 used for rock conductivity experiments in Test 4, and no residue gel breaking fluid was used for
366 rock conductivity experiments in Test 5. Figure 14 showed the rock after conductivity experiment.

Scan Area
Test 4

Scan Area
Test 5

367
368 Figure 14. Damage of proppant embedding to fracture conductivity of a rock sample after test
369 The lowest point on the roughness surface is used as the baseline. Figure 15 showed the surface
370 scan results of the rock surface after the formation water conductivity experiment. Pitting could be
371 seen on the rock and the depth of the pitting was between 0.0791 mm - 0.1780 mm, with most of
372 the pitting depth between 0.09888 mm - 0.1384 mm. Figure 16 showed the surface of the slab
373 after the experiment of no residue breaking. It could be seen that the slag depth of the rock slab
374 was mostly concentrated between 0.1121 mm and 0.3362 mm, and most of the depression depth
375 was concentrated between 0.1494 mm and 0.2988 mm. It was speculated that the slab after the
376 Test 5 experiment was more embedded than the Test 4 due to the potential rock/fluid reaction.
 (A) Laser-scanned image of the fracture surface
(B) statistical map of proppant insertion depth
after the conductivity experiment
Figure 15. Laser scanning imaging of fracture surface and statistical map of depression depth after
formation water conductivity experiment, Test 4

(A) Laser-scanned image of the fracture surface

(B) Statistical map of proppant insertion depth
after the conductivity experiment
Figure 16 Laser scanning imaging of fracture surface and statistical map of depression depth after
formation water conductivity experiment, Test 5
377 3.3.2 Effect of Fracturing Residue on Propped fracture
378 According to the experimental results of 3.2.2, the molecular size of the guar fracturing fluid did
379 not vary much after breaking. As time increased, the amount of residue in the gel breaker
380 gradually increased. Therefore, it was necessary to quantify the residue after the fracturing fluid
381 was broken. The degree of damage to the conductivity was determined, and the damage
382 mechanism of the residue to the conductivity was defined. The steel plate was laid in the
383 conductivity chamber to eliminate the influence of the proppant embedding. 400 ppm of
384 ammonium persulfate was added to the prepared guar gum fracturing fluid, and the flow was
385 tested after breaking the gel at 140 ℃ for 60 mins. The conductivity (Test 6), and the
386 experimental results and the formation water plate conductivity experiment results (Test 1) to
387 calculate the conductivity damage rate, as shown in Figure 17. It could be seen that the gel
388 breaking fracturing fluid containing the residue had a greater damage to the conductivity of the
389 propped fracture and increased with the increase of the closing pressure, and the damage rate
390 increased from 21.7% to 50.6%. This was because the pore volume between the proppants was
391 reduced by 30% to 40% due to the increase in the closing pressure, and the pore diameter between
392 the proppants was reduced from 200 μm to 124.2 μm to 200 μm to 18 μm (Berg, 1970). The
393 macromolecules were more likely to plug in the proppant pores causing an increase in the rate of
394 damage (Hakiki et al., 2015).

395
396 Figure 17. Damage to conductivity caused by the residue of fracturing fluid
397 In order to further study the microscopic adsorption of the residue on the surface of the proppant,
398 the proppant of the formation water diversion experiment Test 1 and the gel breaking fracturing
399 fluid conductivity Test 6 were subjected to SEM electron microscopy and EDS elemental analysis,
400 as shown in Figure 18 and Table 3 & 4. Comparing Figure 18 (A) and (B), it could be seen that the
401 surface of the proppant adsorbed a large amount of a substance similar to the residue, which
402 reduced the porosity between the proppants and caused damage to the conductivity. The EDS of
403 the proppant surface after the Test 1 formation water conductivity experiment showed that the
404 main elementss were aluminuml and oxygen (Table 3), which belonged to the main component of
405 the ceramic proppant, and the proppant surface EDS after the test of the breakage. The results
406 showed that the main elementss were carbon and oxygen (Table 4), which belonged to the main
407 component of guar fracturing fluid, which proved that the residue on the surface of the proppant
408 belonged to the residue of the gel breaking fluid. Therefore, the results of SEM scanning and EDS
409 elemental analysis further verified the damage of the residue to the conductivity of the propped
410 fracture.
 (A) Micromorphology of proppants after formation (B) Micromorphology of proppants after gel
water conductivity Test (Test 1), 200 μm breaking liquid conductivity Test (Test 6), 100 μm
Figure 18. The SEM scanning of proppant microstructure
411
412 Table 3 . EDS element analysis of proppant after gel breaking liquid conductivity test (Test 1)
Element CK OK Na K Al K Si K SK Cl K KK Ca K Mn K Fe K
Weight, % 2.92 44.09 3.52 30.29 4.16 2.16 0.47 0.39 2.12 3.49 6.39
Atomic, % 5.13 58.08 3.23 23.66 3.12 1.42 0.28 0.21 1.12 1.34 2.41
413
414 Table 4. EDS element analysis of proppant after formation water conductivity test (Test 6)
Element CK OK Al K Mn K Fe K Co K Cu K Zn K
Weight, % 27.88 16.73 6.14 5.35 15.61 2.95 12.18 13.16
Atomic, % 52.58 23.69 5.15 2.2 6.33 1.13 4.34 4.56
415 4. Conclusions and Suggestions
416 In this paper, a series of experiments related to fracturing fluid gel breaking and conductivity
417 under high temperature environment were carried out. The effects of the amount of breaker and
418 temperature on the performance of the gel breaking fluid were studied, as well as the damage of
419 the gel breaking fluid to the performance and conductivity of the propped fracture. The main
420 conclusions and suggestions are as follows:
421 (1) The gel breaking performance of the guar gum fracturing fluid is affected by the amount of the
422 gel breaker and the temperature. The excessive amount of the gel breaker and the high temperature
423 conditions cannot effectively reduce the median particle size of the gel breaker. The content of the
424 residue in the mixture also increases, which is mainly caused by the insoluble matter formed due
425 to the residue produced after molecule exceeding solubility limit. The optimum concentration of
426 the breaker at 140 is 400 ppm.
427 (2) When the closing pressure is above 50 MPa, the soaking of the gel breaking fluid on the
428 proppant will significantly increase the crush rate, and the longer the soak time, the greater the
429 damage caused, and therefore the more reduction on conductivity due to proppant crushing; when
430 the closing pressure is below 50 MPa, the proppant crush rate is low, and the impact of the soak of
431 the gel breaking fluid is small. Therefore, in field, the fracturing fluid flowback time should be
432 shortened as much as possible to reduce the soaking effect of the gel breaking fluid on the
433 proppant.
434 (3) The damage of the conductivity caused by the crush and embedding of the proppant showed
435 that the potential rock/fluid reaction between the gel breaking fluid and the formation has a certain
436 influence on the proppant embedding. The laser scanning images showed that the sag depth after
437 the experiment of formation water conductivity was concentrated between 0.09888mm and
438 0.1384mm, which was less than the sag depth of 0.1121 mm - 0.3362 mm after the experiment of
439 no residue breaking. SEM electron microscopy and EDS elemental analysis further verified the
440 damage of the residue to the proppant and conductivity.
441 (4) In summary: the excessive amount of gel breaker and high temperature environment cannot
442 effectively reduce the median particle size of the gel breaking fluid, and the residue content will
443 also increase; the soaking effect of the gel breaking fluid will aggravate the crush and embedding
444 of the proppant, which leads to the decrease of the conductivity. The damage of the residue to
445 conductivity is mainly caused by the residue remaining in the reservoir blocking the channel of the
446 propped fracture.
447 Contributors
448 Special gratitude is owed to Professor Zhou Fujian and Huang Yixiao, post-graduates of
449 Unconventional Oil and Gas Research Institute of China University of Petroleum (Beijing).
450 Professor Zhou Fujian, as the corresponding author of this paper, provided research ideas, funding
451 and laboratory; Wang Jie is the data analysist and main author; Huang Yixiao is the key
452 accomplisher of the laboratory experiment.
453 Notes
454 The authors declare no competing financial interest.
455 Acknowledgments
456 This work is financially supported by the National Science Foundation of China (Grant No.
457 51804033), the National Science and Technology Major Projects of China (Grant Nos.
458 2016ZX05051, 2016ZX05014-005, and 2017ZX05030).
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 Highlights
1. The combination of viscosity, median particle size and residue content is proposed as a criterion
for evaluating whether the fracturing fluid is broken.
2. Gel breaking fluid intensifies proppant crushing and embedding to reduce fracture zone
conductivity.
3. Reveals the mechanism of damage caused by the gel breaking fluid to the fracture.
 Statement of Originality
This work has not previously been submitted for journals. To the best of my knowledge
and belief, the thesis contains no material previously published or written by another
person except where due reference is made in the thesis itself.
Jie Wang Nov 2019